Every month for a year, samples of aromatic bitters stored in clear and green bottles under conditions relevant to the retail trade, (1) in sunlight, (2) in fluorescent light and (3) in the dark, were characterized by descriptive sensory analysis, tristimulus colorimetry and by the concentrations of 13 flavour compounds. Aromatic bitters stored in light developed a higher intensity of sweet and solvent-like odour, described by the assessors as catty-like or ribes. Bitters stored in light had a stronger tendency to become turbid and these samples had a fortified-wine-like flavour and were less bitter and less astringent. A new method in this context, growth curve analysis, was used successfully to detect significant time and treatment effects in the sensory data. By partial least-squares analysis only a minor part of the light-induced sensory effects in bitters could be accounted for by the concentration of flavour compounds.

Studies were carried out to determine the effect of baking, in different types of oven such as an earthen tendoor, a gas tandoor, an electric oven and a heated plate, on the physico-chemical and quality characteristics of tandoori roti. The studies indicated that the extent of gelatinization of starch varied depending on the type of oven used and was found to be 74.6, 78.4, 90.7 and 88.4% in roties baked in an earthen tandoor, a gas tandoor, an electric oven and a heated plate respectively. The pasting characteristics of starch, separated from the tandoori roti sample and measured using a Rapid Visco Analyzer, indicated the highest peak viscosity (36 SNU) for tandoori roti baked in an earthen tandoor and the lowest (25 SNU) for that baked in an electric oven. The concentration of high molecular weight proteins was lower in roti baked in an earthen tandoor and a gas tandoor, indicating greater dissociation of high molecular weight proteins during baking in such ovens. The sensory texture, taste and flavour of roti baked in an earthern tandoor was found to be superior to those baked in other types of ovens.

The combination of the relative abundances of carbon and nitrogen isotopes (δ¹³C- and δ¹⁵N-values) in fruit juice pulps led to characteristic clusters, on the basis of which regional origin assignments of citrus juices were possible, which would not have been attained on the basis of only one of these parameters. Thus, while the δ¹³C-values of juice pulps from Italy partially overlapped with those from Brazil, the δ¹⁵N-values permitted an origin assignment. First attempts to extend this multi-isotope analysis to a multi-compound¹⁵N analysis, by correlating the δ¹⁵N-values of fruit juice pulps to those of free amino acids, were promising. The results obtained were in line with general observation on¹⁵N abundances and biochemical correlations of secondary plant products.

The levels of 13 polycyclic aromatic hydrocarbons (PAH) were determined by an HPLC method with fluorescence and UV detection and by a GC/MS technique in smoked fishery products from modern smoking kilns with external smoke generation and from traditional smoking kilns. The average benzo(a)pyrene (BaP) concentration of all 35 samples from commercial smoking kilns with external smoke generation was 0.1 μg/kg (wet weight) and the sum of the carcinogenic compounds determined in the study, i.e. benz(a)anthracene, chrysene, benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(a)pyrene, dibenz(a,h)anthracene and indeno(1,2,3-c,d)pyrene did not exceed 4.5 μg/kg (wet weight). The BaP levels of the 27 smoked fish samples from traditional kilns ranged from 0.2 μg/kg to 4.1 μg/kg, with a mean value of 1.2 μg BaP/kg. The average concentration of the sum of the carcinogenic compounds was 9.0 μg/kg. Large variations were found in the content of the non-carcinogenic PAHs phenanthrene, anthracene, fluoranthene and pyrene in all samples from both types of smoking kilns.

A comparative study of methods for isolating cell wall material from olives (variety Hojiblanca) was performed. Treatment with cold (T-1) or hot (T-2) ethyl alcohol was followed by extraction into cold or hot water (water-soluble fraction). The insoluble residues were delignified. Hemicelluloses A and B were isolated and the neutral sugar composition and protein content of the different fractions were determined. In the delignified fractions following treatments T-1 and T-2, hemicelluloses A were composed of 87.35% and 87.37% xylose, respectively, indicating the presence of a pure xylan. In the non-delignified fraction, the content of hemicelluloses B was higher than in the delignified fraction and its predominant sugar was glucose, although significant amounts of xylose, galactose and arabinose were also found. The study suggests that treatment T-1 gives better results than T-2 and that a higher degree of purification of hemicelluloses A is obtained from the delignified cell wall material, as well as a decrease in the proteins bound to the fractions.

The inhibitory effects of clove, cinnamon, cardamom, turmeric and pepper on the histamine production and histidine decarboxylase activity ofMorganella morganii (a potent histamine-producing bacteria in fish) was examined at 30°C using HPLC. Cinnamon and clove exhibited a significant (P<0.01) inhibitory effect, whereas turmeric and cardamom had a moderate effect. These spices were applied to whole mackerel at a level of 3% and their inhibitory effect on biogenic amine formation at 30°C was also examined. As in the in vitro study, clove and cinnamon showed a significant (P< 0.05) inhibitory effect on histamine, putrescine and tyramine formation but not on that of cadaverine. Cardamom and turmeric exhibited a moderate effect and pepper was ineffective. Therefore, clove and cinnamon are more helpful than cardamom and turmeric in the minimization of the formation of toxic histamine in mackerel.

Investigations into the sources of contamination of virgin olive oil by gasoline components were concluded. Olives on the tree contained volatile aromatic hydrocarbons at concentrations exceeding those corresponding to the equilibrium with the environment. Present knowledge indicates that up to 10 μg/kg of benzene and 250 μg/kg for the sum of benzene, toluene, and the C₂-benzenes must be considered as possible background concentrations. Aside from the oil mills, the rooms for intermediate storage of the olives were found to be an important source of contamination by gasoline vapours, since they often contain vehicles and other gasoline-driven engines. Parking of a small, hot grass mower into a similar room released an amount of gasoline that was sufficient to contaminate the oil in olives above the proposed limit by a factor of 100. Recommendations are derived for the producers to avoid contamination of olive oil with gasoline components.

For the determination of organochlorine pesticides (OCPs) in vegetable oils and oil seed samples, a solid-phase extraction method is described, modified from that developed by Steinwandter, with silica gel columns activated with a 10% water content. In comparison to the method developed by Steinwandter, we reduced the amount of solvents and chemicals required for sample preparation and substituted dichloromethane by the much less toxictert-butylmethyl ether in the eluent mixture. In this manner the sample preparation technique becomes more convenient, cheaper and ecologically more justifiable. Under the specified sample preparation and elution conditions 1 g silica gel retained about 16 mg triglycerides whereas the OCPs were quantitatively eluted. The recoveries for hexachlorobenze, (HCB) α-HCH, Lindane (γ-HCH) γ-HCH, Heptachlor, Heptachlorepoxid,o,p′-DDE,p,p′-DDE, Dieldrin,o,p′-DDT,p,p′-DDT were between 75 and 90%. The reproducibility of the total method was excellent as well as its ruggedness.

Pomegranates cv. “Mollar” were stored for up to 8 weeks at 5 °C and above 95% relative humidity (RH) in air and in controlled atmospheres of 10% O₂ and 5% CO₂, 5% O₂ and 5% CO₂, 5% O₂ and 0% CO₂ and 5% O₂ and 0% CO₂ ethylene-free. Storage was followed by a shelf-life period of 6 days at 20 °C in air. Respiratory activity slightly declined during storage at 20 °C, from 12 to 8 ml CO₂ · kg⁻¹ · h⁻¹ and was around 4 ml CO₂ · kg⁻¹ · h⁻¹ at 5 °C showing a non-climacteric pattern. When compared with color at harvest, an increase in thea^* value in the juice from pomegranates stored in 10% O₂ and 5% CO₂ was observed. This supports that view that juice red colour can increase in intensity during storage. Controlled atmosphere storage reduced weight loss, the risk of decay and the severity of husk scald (except at 10% O₂ and 5% CO₂). The relatively low control of husk scald at 5% O₂ disagrees with the level proposed previously for “Wonderful” cv.; “Mollar” cv. seems to be more sensitive to scald than other varieties. No symptoms of black spots or membranose and no off-flavours were detected at any time. However after a period of shelf-life storage, the controlled atmosphere caused a slight reduction (lower than in air-stored fruit) in titratable acidity, reducing sugars and vitamin C and an increase of the soluble solids content/titratable acidity (maturity index) without differences among the various gas compositions studied. The maturity index must be considered to be a good criterion of pomegranate maturity for sweet varieties.

Semi-hard ewe's milk cheeses, frozen immediately after manufacture either slowly at −35 °C or rapidly at −80 °C and stored at −20 °C for 4 months were studied for microstructural and textural characteristics during subsequent ripening. Two control groups were used to establish the effect of freezing: the fresh unfrozen cheese and cheese thawed immediately after freezing. Freezing proper did not result in any marked changes in the textural parameters of the cheeses, but considerable changes were found in slowly frozen cheeses after 4 months of frozen storage. Shear strength values were lower in all frozen and stored cheeses, particularly in cheese samples frozen slowly compared to those in the unfrozen control batch. This parameter and firmness values were significantly lower in both slowly and rapidly frozen cheeses at the completion of ripening. Ripening tended to offset differences in elasticity, noticeable in the cheeses during the first 30 days of ripening. Light microscopy and electron microscopy revealed small cracks and ruptures in the cheeses which could not be observed by the naked eye. More extensive damage to the cheese microstructure was found in slowly frozen cheese samples stored frozen for 4 months.

In order to find out biochemical markers for the botanical origin of heather (Erica) honey, the phenolic metabolites present in heather floral nectar, collected from the honey-stomach of bees gathering nectar from these flowers, were analysed. The flavonoid fraction of nectar contained four main flavonoids. Two of them were quercetin and kaempferol 3-rhamnosides, and the other two were tentatively identified as myricetin 3′-methyl ether and isorhamnetin 3-rhamnosides. Since the natural glycosides are hydrolysed by bee enzymes to render the corresponding aglycones, which are the metabolites detected in honey, acid hydrolysis of the nectar glycosides was achieved. The aglycones quercetin, myricetin 3′-methyl ether, kaempferol and isorhamnetin were identified, as well as the gallic acid derivative ellagic acid. The analysis of Portuguese heather honey samples showed that ellagic acid was present in all the samples in significant amounts ranging between 100 μg and 600 μg per 100 g honey. The other nectar-derived flavonoids were also present, although some of them in very variable amounts. Ellagic acid and myricetin 3′-methyl ether, which have not been detected in any of the monofloral honey samples investigated so far, with the only exception being a French honey sample of the botanically relatedCalluna (Ericaceae) which also contained ellagic acid, seem to be the most useful potential markers for the floral origin of heather honey. However, more detailed and extensive investigations are needed to prove the utility of these markers.

The rheological behaviour of meat batters during heating was analysed as a function of protein level (10–16%), type (pork back or perirenal/peritoneal fat) and amount (10–22%) of fat used. Fat thermal behaviour was studied by differential scanning calorimetry and rheological properties of batters were assessed using non-destructive measurements (thermal scanning rigidity monitor). The higher the protein content, the higher were the rigidity values displayed by the batters, irrespective of fat type, although the magnitude of these values appeared to be dependent on the amount and characteristics of the fat. The lower the fat content, the lower were the rigidity values of the batters. This behaviour pattern was influenced by the amount of protein present. In general, samples containing perirenal/peritoneal fat exhibited lower rigidity values at high temperatures, whereas at less than 35–40 °C, the opposite appeared to be the case.

Response surface methodology was used to determine the role played by egg white and starch in gelation of minced and washed sardine muscle. There was no detectable interaction, either positive or negative, between the effects of the two ingredients. Both egg white and starch significantly affected gel strength. Egg white had a direct, positive influence on hardness and adhesiveness. Starch had a direct, positive influence on cohesiveness and the ability to retain water.

Cereal varieties cultivated in Germany, such as wheat, rye, grain-maize, barley, and oats were analyzed for fumonisins, including also imported maize from Argentina. In a total of 410 wheat samples and 140 rye samples of two harvesting years (1993, 1994) and in random samples of barley and oats no fumonisins were detected at all. In german grain-maize of 1993, only low fumonisin contents (17–33 ng/g) were detected occasionally. Some grain-maize samples of the 1994 harvest contained significantly higher fumonisin amounts, partly up to the mg/kg-range, which obviously is due to the extremely high temperatures during summer. In some samples of variety tests of the country the fumonisin B₁ content amounted up to 4828 ng/g and the total fumonisin content (FB₁-FB₃) up to 7132 ng/g respectively. In 1994 a total of 317 native grain-maize samples was tested, of it 109 samples of German cultivation and 208 samples from variety tests of different federeal states. Maize samples from Baden-Württemberg, which are representative to the maize harvest of this state, had a fumonisin contamination of 14%, the mean value of the contaminated samples amounting to 206 ng/g. Of the imported maize from Argentina, all the investigated 21 samples had a fumonisin content (FB₁-FB₃) of 14–1106 ng/g, the mean fumonisin content amounting to 175 ng/g.

Solid phase extraction (SPE) with the porous carbon sorbent CARB GR was used for the preconcentration of metalaxyl residues from a variety of Slovak grape wines with subsequent capillary GC and GC/MS analysis. Recovery was tested at various concentrations of metalaxyl in standard solutions (recovery,R≥92%, relative standard deviation RSD≤4.3%) and in wines. The value of recovery in spiked wines was dependent on the concentration (studied in the range 0.02–1.96 mg/1) and on the variety of wine (R=80–99%; RSD=2–7%). Limits of quantitation (for a sample volume of 50 ml) were determined to be 0.75 μg/1 with GC-FID and 0.50 μg/1 with GC/MS-ITD. Concentration levels of metalaxyl residues were determined in treated wines (with 0.25% Ridomil plus 48 WP) and a strong dependence on the protective term before the harvest was shown.

Margarines and shortenings available in Austria were repeatedly sampled in 1991/1992 and the content oftrans fatty acids (TFA) determined by using capillary GLC. Wide variations of the TFA contents with respect to intra- and inter-brand differences were observed. Diet margarines contained up to 1% TFA, while TFA concentrations in tub or stick margarines were much higher (15.7±5.8% and 21.3±5.3%, respectively). A sub-set of samples was also purchased in 1995 and a general reduction of the TFA content was noticed. Taking into account different market shares of certain margarine types, a weighted average of 15.7% TFA and 6.5% TFA was calculated for the 1991/1992 and the 1995 samples. Based on availability data the amount of TFA supplied with margarines was estimated to be 3.7 g per person per day, while a more accurate method of measuring dietary intakes, i.e. diet history and food frequency data, approximates the amount of TFA supplied with margarines to be 1.5 g per person per day for the 1991/1992 samples and 0.6 g for the 1995 samples.

The quantitative determination of total phenols, ellagic tannins and gallic and ellagic acids in the peel of the Tunisian pomegranate variety Chelfi, has been carried out. The ellagic tannin content is prominently less than the amount of total phenols, which led us to look for the presence of the condensed tannins. The determination of the content of catechic tannins in eight Tunisian varieties of the pomegranate was carried out using weekly samples over a period of 2 months.

A fast breakdown of glycogen is observed in muscles of stress-susceptible pigs leading to pale, soft and exudative (PSE) meat. We report a comparative study of pyruvate kinase from muscles of normal and PSE-prone pigs. Compared with the enzyme from normal muscle, pyruvate kinase isolated from PSE muscle shows a five times lower Michaelis constant,K_m, for phosphoenol pyruvate and a more than ten times higherk_cat/K_m value. The pH dependency of the enzymatic activity is shifted to more acidic values for pyruvate kinase from PSE muscles. According to isoelectric focusing, pyruvate kinase from PSE muscle consists of three isoforms, while only two isoforms are detectable in pyruvate kinase preparations from normal pigs. The various isoforms were isolated by preparative isoelectric focusing and their steady-state properties were compared. Isoform 3, which is found only in PSE muscle, shows a 10-fold higher specific activity, a 30-fold lowerK_m value and a 100-fold increasedk_cat/K_m value for phosphoenol pyruvate as compared to isoform 1. The presence of isoform 3 in PSE muscle appears to be responsible for the high activity of this enzyme under the more acidic conditions prevailing in PSE muscle. In vitro phosphorylation and dephosphorylation experiments using total enzyme and purified isoenzyme 1 suggest that isoforms 2 and 3 arise from isoform 1 by phosphorylation. Thus protein phosphorylation seems to be responsible for the shift in activity of pyruvate kinase, a key enzyme of glycolysis, under the acidic conditions of PSE muscles.

Pumpkin (Cucurbita pepo L.) seed oil is a common salad oil which is produced in the southern parts of Austria, Slovenia and Hungary. It is dark green and has a high content of free fatty acids. Due to its colour, the oil cannot be used for cooking. The content of vitamin E, especiallyγ-tocopherol, is very high. The oil content of the pumpkin seed is about 50%. The seed itself can be eaten. Therefore a pumpkin variety with high vitamin E content is desirable. The aim of this work was to find a variety ofCucurbita pepo which has a high oil yield and a high vitamin E content. A total of 100 breeding lines were tested for their tocopherol content. The tocopherols and tocotrienols are extracted with hexane and analysed by NP-HPLC/FLD with hexane/dioxan (96/4) as eluent, with fluorescence detection at 292/335 nm. The/gg-tocopherol content, which is about 5–10 times as much as that of α-tocopherol varies over a broad range (41–620 mg/kg dry pumpkin seeds).β- andδ-tocopherol are found at low levels.

Ethanol pre-treated apple parenchyma cells are dried in a laboratory vacuum dryer. Various ethanol contents (75 to 95% m/m) and moisture contents (2 to 15 g ethanol-water-mixture per g dry mass) of the cells were adjusted before drying and the influence of these factors on drying behaviour as well as the related structural changes are studied. The initial ethanol content was found to have a significant influence on both, drying behaviour and macrostructure of the dried material. In the case of a low initial value, the ethanol content during drying already drops at moisture contents of about 0.5–1.5 g/g. As a consequence the residual particle moisture consists mainly of water at the end of drying. In contrast to high initial ethanol contents, cells at a low initial ethanol content become strongly deformed on drying. The porosity of the dried material also decreases in the latter case, relatively large and stable aggregates are formed and the water binding capacity of the dried product has diminished on a large scale. The initial moisture content influences the drying behaviour especially on applying low initial ethanol contents. If the initial moisture content is reduced the drop of the ethanol content is shifted towards the end of the drying process. The influence of initial moisture content on macrostructure, however, was found to be small compared with the effect of the initial ethanol content.

Peptides inhibitory to the 70-kDa endopeptidase (PepO) from the cytoplasm ofLactococcus lactis ssp.lactis MG1363 were isolated from the supernatant (pH 4.6) of chymosin, tryptic and α-chymotryptic hydrolysates ofβ-casein (β-CN) by reversed-phase HPLC and identified by sequencing and mass spectrometry. Chymosin releasedβ-CN f193–209, kinetic constant (K_i) of which for inhibition of PepO was 60 μM. This peptide also inhibited (K_i=1700 μM) the 95-kDa aminopeptidase (PepN) fromL. lactis ssp.lactis MG 1363. Trypsin released two PepO-inhibitory peptides: one,β-CN f69–97, was not degradable by PepO (K_i=4.7 μM), while the other,β-CN f141–163, was degradable by PepO but competitively inhibited hydrolysis of methionine enkephalin by PepO. A peptide,β-CN f69–84, which inhibited PepO with aK_i of 8.1 μM, was isolated from the α-chymotryptic hydrolysate. Peptides released fromβ-CN by trypsin or chymotrypsin had very little inhibitory activity against PepN. PepO degradedβ-CN f193–209 very slowly compared with the hydrolysis of methionine enkephalin. All four inhibitory peptides (β-CN f193–209, f69–97, f69–84, f141–163) were readily degraded by thermolysin.

Rehydrated material with cellular structure and alcohol insoluble substance may be regarded as concentrated suspension with viscoelastic properties. The rheological properties of disperse systems are determined on the basis of the material properties of the disperse phase apart from its concentration. The material properties of the disperse phase depend on the macrostructural parameters of the particles including the interactions occuring and the chemical structure of the cell wall. The material properties of the rehydrated material with cellular structure may be detected by means of classical rheological examinations and specifically systemizing their evaluation. The description of material with cellular structure with the aid of CASSON's model and the further investigation of the yield stress τ0 as a function of its concentration and of the effektive viscosity η_eff as a function of its concentration and shear rateγ seem to be established. If comprehensivly applied this method allows to interpret the rheological properties of the material with cellular structure in specific respect. The dominant linear dependence of the influencing variables yield stress, CASSON's viscosity and effectiv viscosity on concentration is especially remarkable.

A method for the determination of D-malic acid in products of fruits is presented. After addition of undecanoic acid as internal standard the dehydrated sample is extractive methylated by conc. hydrochloric acid, methanol and anhydrous magnesium sulfate. The extract is subjected to gaschromatographic separation on a chiral phase. Quantification of D-malic acid is done by the method of standard addition. The relative standard deviation is in the range of 1,8–4,4%, the detection limit 2,1–2,7 mg/l, the limit of quantitation 3,6–4,1 mg/l. Measures of fruit juice, fruit wine, wine and vinegar are tabulated.

A simplified and improved method is described for the preparation of pyrraline, a lysine derivative from the advanced Maillard reaction and potential indicator for heat treatment of foods. The compound was obtained in a high degree of purity and with a yield of 31% fromN^α-t-butyloxycarbonyl-L-lysine after heating with 3-deoxy-D-erythro-hexos-2-ulose for 2 h at 70°C in the dry state, preparative fractionation of the resultingN^α-t-butyloxycarbonyl pyrraline with reverse-phase liquid chromatography and final deprotection of the intermediate compound with acetic acid.

The changes in the quality parameters of Spanish pomegranate fruit (cultivar Mollar) during ripening and during 7 weeks of cold storage at 5°C and 90–95% relative humidity were studied. The fruit and seed weights, as well as the surface colour increased with ripening. Total soluble solids (TSS), pH and titratable acidity (TA) did not show significant differences during the weeks studied (from the 26th to 32nd weeks after flowering), but the seeds' colour (“Lab” values) and juice colour (absorbance at 510 nm) showed an increase during this period with a maximum during the last 2 weeks. These results indicate that pomegranates should be harvested during the 31st to the 32nd after flowering, in order to get the best pigmentation without a decrease in other quality parameters. The anthocyanin profile changed during the different maturity stages, since the diglucoside derivatives were the prevailing pigments during the early ripening stages, whereas the monoglucoside derivatives were the main pigments in the latter stages. After cold storage of pomegranates harvested at two maturity stages, no differences in TSS, pH, TA and skin colour were observed. In addition, seeds' and juice colour did not decrease during storage. Hence, this study supports the theory that pomegranate is a nonclimacteric fruit and that pomegranates can be stored for at least 45 days without deterioration in the fruit quality.

Food-grade PVC film containing 28.3% dioctyladipate (DOA) plasticizer was used to wrap chicken meat samples, with and without skin, contained in a polystyrene tray. Samples were then irradiated with γ-radiation [⁶⁰Co] at doses equal to 4 kGy and 9 kGy corresponding to “cold pasteurization”. Irradiation was carried out at 8–10 °C and samples were subsequently stored at 4–5 °C. Contaminated chicken meat samples were analysed for DOA at intervals between 7 h and 240 h of contact, using an indirect GC method. Identical non-irradiated (control) samples were also analysed for their DOA content. Results showed no statistically significant differences in migrated amounts of DOA between irradiated and non-irradiated samples. Neither were differences observed between samples irradiated at 4 kGy and 9 kGy. This was supported by identical IR spectra recorded for irradiated and non-irradiated samples and leads to the conclusion that, at such intermediate radiation doses (⩽kGy), the migration characteristics of PVC film are not affected. DOA migration was found to be time dependent, approaching equilibrium after approximately 170 h for the chicken flesh plus skin samples and 120 h for the chicken flesh samples. The amount of DOA migrated into chicken flesh plus skin samples was significantly greater (3.2–22.3 mg/dm²) than that for chicken flesh samples (0.9–8.9 mg/dm²). After 240 h of sample/ film contact under refrigeration, loss of DOA was approximately 35.6% for chicken flesh plus skin samples and 14.3% for chicken flesh samples. Sample spoilage, as demonstrated by off-odour development, occurred after approximately 120 h of refrigerated storage. Diffusion coefficients for DOA were calculated and were found to be lower for chicken flesh (1×10⁻¹³) than for flesh plus skin (4.4×10⁻¹³) samples.

Most parts of Germany are iodine deficiency areas. Daily iodine intake may be increased by food with high iodine content. Therefore determination of iodine in different foodstuffs is of importance. Aim of our work was to develop a method for mineral waters. Besides, we wanted to find out to what extent natural mineral waters can contribute to the iodine supply of the population. The method is based on the reaction of the halogenids iodide and bromide with ethylene oxide in a sulfuric acid medium while converting into 2-iodo- and 2-bromoethanol. After extraction, the reaction products are determined by capillary gas chromatography with an electron capture detector. The method was modified for mineral waters. Single results were confirmed by ICP-MS. For mineral waters the limits of determination are 3 μg/L for iodide and 42 μg/L for bromide. The investigation of mineral waters from Hessen showed, that only few sources contain iodide in remarkable amounts. Therefore a considerable improvement of iodide intake is possible only with single mineral waters.

A complete mobilization of veterinary drug residues for quantitative analytical detection is often unsuccessful. For some drugs, one reason for this is the quite different binding forms between the drug and the food matrix, which for three groups of veterinary drugs may be described by sorption-isothermals. The influence of gluta-thione on sorption-isothermals and residue mobilization is discussed. Thus, better interpretations regarding the availability of residues are possible.

The essential oil from guarana [Paullinia cupana H.B.K. var. sorbilis (Mart.) Ducke] was analysed. Nine components were identified, namely (2) methylbenzenes, (1) cyclic monoterpene and (2) cyclic sesquiterpene hydrocarbons, (2) methoxyphenylpropenes and (2) alkylphenol derivatives. The alleged psychoactivity of the essential oil is presumably due to the identified constituents estragole and anethole. Any contribution of aminated metabolites of estragole/anethole to the alleged psychoactivity of the essential oil of guarana can be excluded. Neither the psychoactive 4-methoxyamphetamine nortert-aminoketones could be traced in human urine after oral application of guarana.

Enantioselective gas chromatography using heptakis (6-0-tert.-butyldimethylsilyl-2,3-di-0-methyl)-β-cyclodextrin as the chiral stationary phase was used in chirality evaluation of ethyl lactate in wines, which is helpful in the quality assurance of wine. (S)-methyl lactate is recommended as an internal standard.

The paper deals with the contamination of human milk with chlorinated phenols. The average and median concentrations of the chlorophenols investigated ranged from 0.75 to 9.74 μg.kg⁻¹ and from being not detectable to 5.62 μg.kg⁻¹, respectively, for the different compounds. The highest average and median levels were found for pentachlorophenol and 2,4,5-trichlorophenol. The concentrations determined were below the permissible levels.

Migration of dioctyladipate (DOA) and acetyltributylcitrate (ATBC) plasticizers from plasticized Polyvinylchloride (PVC) and polyvinylidene chloride (PVDC/PVC (Saran) films into both olive oil and distilled water during microwave heating has been studied. The plasticizer migrating into olive oil and water was determined using an indirect GC method after saponification of the ester-type plasticizer (DOA or ATBC) and subsequent collection of the alcohol component of the ester, namely: 2-ethyl-1-hexanol and 1-butanol, respectively. Migration was dependent on heating time, microwave power setting, the nature of the food simulant and the initial concentration of the plasticizer in the film. Migration of DOA into olive oil reached equilibrium after heating for 10 min at full power (604.6 mg DOA/1). Migration into distilled water was 74.1 mg/1 after 8 min of microwave cooking at full power. The amount of ATBC migrating into olive oil reached equilibrium after heating for 10 min at full power (73.9 mg ATBC/1). Migration into distilled water was 4.1 mg/1 after heating at full power for 8 min. Control samples containing olive oil gave DOA migration values which were significantly higher than the upper limit for global migration (60 mg/1) set by the European Community. It is proposed that PVC should not be used in direct contact with food in the microwave oven, while Saran may be used with caution in microwave heating and reheating applications, avoiding its direct contact with high fat foodstuffs.

The sensory intensity measured as theabsolute threshold value of spice andrecognition of spice was evaluated for summer savory and rosemary in meat balls. The values forabsolute threshold value of spice were found to be significantly lower for rosemary than for summer savory. The antioxidative activity of the spices was analysed in two accelerated model systems and in a storage experiment. In one of the model systems, oxidation was accelerated by heat and by an elevated pressure of oxygen. Both spices significantly improved the oxidative stability of the meat balls in this model system. In the second model system metal catalyst oxidation in a meat slurry was used and a reduction in the oxidative processes in samples containing the spices was again shown. In both model systems a slightly higher antioxidative activity was seen for rosemary compared to summer savory. In the storage experiment, the spices were added at a sensorially acceptable level and the heat-treated meat balls were stored at 5°C. A significant reduction in the development of warmed-over flavour (WOF) caused by the addition of spices was measured by a reduction in 2-thiobarbituricacid-reactivesubstances (TBARS) and in hexanal. A reduction in TBARS of approximately 30% in meat balls containing added spices was seen independently of packaging in 1% oxygen or in atmospheric air and the reduction (30%) was constant throughout the storage period.

The effects of natural fermentation upon phytic acid and less phosphorylated inositol phosphates ofLens culinaris var vulgaris cultivar Magda-20 were investigated. Seven fermentation runs were made following a 2² complete factorial design with three replicated centre points to study the effect of different conditions of temperature (28, 35 and 42°C) and broth concentration (79, 150 and 221 g/l). Samples were taken for each of them at daily intervals (0, 24, 48, 72 and 96 h). The pH value declined sharply in the first 24 h of fermentation, becoming stabilized from this time. The relation between lactic acid and titratable acidity presented important differences between the different fermentations, ranging from 30–80%. Phytic acid (IP₆), inositol pentakis (IP₅), tetrakis (IP₄) and tris-(IP₃) phosphates were quantitatively determined. The content of total inositol phosphates showed a maximum reduction of 63% at 72 h under the fermentation conditions of 42°C and 79 g/l.

Irradiation combined with a conventional cooking procedure was applied to meatball and the effects on bacterial load and inoculatedAeromonas hydrophila were determined. Meatball samples were irradiated by using a⁶⁰Co source at the dose levels of 0, 0.30,0.75,1.50,2.50 kGy and cold stored at 4±1°C for 7 days. Bacterial load and the count ofA. hydrophila decreased when the irradiation dose level increased. A minimum inhibition effect was found at the dose of 0.30 kGy. Irradiation in combination with a conventional cooking procedure was found to be more effective in reducingA. hydrophila and the bacterial load in meatball. This study indicated that a dose of 0.75 kGy was sufficient to destroy approximately 10⁴ cfu/g ofA. hydrophila in meatball.

We have established an electrophoretic method to evaluate proteolysis in Parmesan cheese by means of an objective ripening index. The separation of caseins by alkaline polyacrylamide gel electrophoresis (PAGE) (12% T, 2.6% C, pH 8.9, 5 M urea) is followed by the densitometric analysis of theγ- andβ-casein fractions. The relationship between the resulting coefficients (γ-Cn/β-Cn) and the age of reference samples of Original Italian Grana Padano (6–22 months) was linear up to 15 months, allowing an evaluation of the extent of proteolysis and therefore a deduction of the age of the Parmesan samples analysed. Based on this calibration we propose to use a threshold level of 1.3 (γ-Cn/β-Cn) to verify the required age, i.e. 12 months, of Parmesan cheese, retailed as a loaf or prepacked slices. Commercially grated Parmesan samples may contain ≤20% cheese rind, which has a very low degree of casein breakdown. So a threshold level of 0.8 (γ-Cn/β-Cn) is proposed for all grated Parmesan products. The preparation of reference solutions with defined coefficients (γ-Cn/β-Cn), corresponding to the proteolysis indices of reference samples of different aged Grana Padano is described. The coefficients (γ-Cn/β-Cn) as well as theβ-casein content of two additional series of reference samples and of 49 commercial Parmesan samples taken from retail outlets in Austria and Italy are presented.

Free sugars have been determined by HPLC in fresh pineapple fruit, freshly extracted pineapple juice (home-made), pineapple juice concentrate (for industrial use), commercial pineapple juices and nectars. In natural samples, intermediate products and commercial juices the dominant sugar was sucrose, followed by fructose and glucose, both of which were found in similar concentrations. However, the sugar content of nectars analyzed was highly variable. The presence of maltose in nectar samples is a clear indication of the addition of sugars from corn syrup. We have found a fructose/glucose ratio close to 1, and the coefficient fructose plus glucose/sucrose close to 1, both of which are a good index of authenticity of pineapple juices.

This study describes the accelerating effect exerted on proteolysis and flavour development in cheese-curd slurries by combined application ofLactococcus lactis subsp.lactis IFPL359 and high concentrations of its Lac⁻ Prt⁻ derivative, (i.e. that which has reduced capacity to metabolize lactose and reduced proteolytic activity, strain T1). Cells of strain T1 partially lysed by either sonication or incubation with lysozyme, were also used to ascertain how proteolysis was affected by release of intracellular enzymes in the initial stage of incubation of the strains in cheese-curd slurries. The presence of strain T1 produced higher levels of non-protein nitrogen (NPN) and amine nitrogen (AN) during the first weeks of incubation when partially lysed cells had been added. Addition of whole cells of strain T1 produced higher values of NPN and AN at the end of incubation of slurries, accelerating proteolysis by about 2 weeks with respect to the control, which only contained the parental strain IFPL359. At the end of the experimental period higher amino acid levels were detected by HPLC in the slurry containing whole T1 cells. Volatile fractions of the different cheese-curd slurries were also analysed. The higher level of proteolysis produced by addition of high levels of strain T1 appeared to be related to release of intracellular enzymes by this strain owing to its greater capacity for autolysis.

The following substances were evaluated as potent taste compounds: acetic acid, propionic acid, lactic acid, succinic acid and glutamic acid, each in free form and/or as ammonium, sodium, potassium, magnesium and calcium salts, as well as the corresponding chlorides and phosphates. Magnesium and calcium propionate mainly caused the sweetish note in the taste profile of Emmentaler. Although bitter tasting amino acids and peptides occurred in the cheese sample, they were not detected in the taste profile.

Insoluble deposit formed in aromatic bitters produced from alcoholic extracts of about 30 different botanical materials with a dry matter content of 1.67% and 38 vol% alcohol and a characteristic astringent flavour was shown by¹³C NMR spectroscopy to be a coprecipitate of plant polyphenols, proteins and carbohydrates. The polyphenols in the deposit were flavonoids such as anthocyanidins and anthocyanins, with glucose as the principal carbohydrate and derivatives of cinnamic acid. The deposit formation in the aromatic bitters was accelerated by addition of the radical initiator 2,2′-azobis(2-amidinopropane) dihydrochloride or by addition of hydrogen peroxide in combination with iron(III) nitrate and ascorbic acid as a Fenton reagent. Polymerization of catechin and pelargonidin was shown, in model experiments, to be oxidative and to be accelerated by exposure to light. A mechanism involving oxidative polymerization of polyphenols followed by coprecipitation of polymerized polyphenols, proteins and carbohydrates is proposed for formation of deposits in alcoholic beverages of the bitters type.

An account is given of the application of thermospray LC-MS in the analysis of caffeoyl- andp-coumaroylquinic acids, theaflavins and thearubigins in black tea. All compounds, except for the thearubigens, could be detected as the pseudo-molecular ion [M+H]⁺. In addition to [M+H]⁺, other species such as adducts with sodium, ammonium and potassium, as well as solvent clusters were observed. The formation of those adducts depended upon on the structure of the compound. A fragmentation of chlorogenic acids occurred at elevated temperatures yielding the constituents of the molecules (caffeic,p-coumaric and quinic acids).

Aqueous liquid smoke produces a brown layer on the wall of the polythene receptacle in which it has been contained. The constituents of this brown layer have been extracted using dichloromethane and were studied by means of gas chromatography/mass spectrometry (GC/MS) and Fourier transform infrared spectroscopy (FTIR). Some changes in the liquid smoke were deduced through comparisons of data from the brown layer with the previously obtained liquid smoke data. Due to interactions between polythene molecules and compounds of the liquid smoke, some of these latter compounds migrate into the wall of the receptacle and are retained there. The extent of these migrations depends on the size of the hydrocarbon part of each compound. However, far from being harmful, this migration is useful, since compounds irrelevant from the point of view of flavour, and harmful to health are the main compounds affected by the retention on the polythene wall. Some of the adsorbed compounds have not previously been reported to be present in liquid smoke.

The main purpose of this work was to evaluate the colouring effect of carotenoids present in dry biomass obtained from stressed cells ofChlorella vulgaris. Total carotenoids represented only 0.2% of dry algal biomass and consisted mainly of canthaxanthin, lutein, astaxanthin and their esters. — A rainbow trout feeding trial was conducted in order to investigate the effects of dietary algal incorporation as a pigment source, in comparison to that obtained with synthetic pigments, both astaxanthin and canthaxanthin. — The colour intensities measured in muscle were compared, in each case, with those which constitute the Salmonids Roche Colour Card, and proved similar after both 3 and 6 weeks feeding, with a significant increase detected, but at the end of experiment (9 weeks) the increase was shown only in spectrophotometric (quantitative) results.Chlorella vulgaris biomass, which is storable without any special precautions, thus appears to be a promising source of carotenoids to use in commercial fish finishing diets, quite comparable in efficiency with the existing synthetic pigments. Algal biomass micronization, which was also tried out, was not found to be advantageous for the efficiency of colouring, no evidence having been found of any difference in its absorption and in the distribution of pigment through muscle, even if a 150-g rainbow trout, which has a rather short digestive tract, was used.

Three methods for evaluation of gas Chromatographic data have been compared. Multiple linear regression (MLR) as developed by Precht, principal component regression (PCR) and partial leastsquares regression (PLS) have been applied to the detection of foreign fat added to pure butter fat samples obtained from several European countries. The emphasis was put on building a calibration model for the general detection of foreign fat and therefore only one was built for the quantitation of various vegetable oils and lard MLR, as developed for German butter fat, was found to be appropriate also for the detection of the addition of about 3–5% foreign fat depending on the formula used. PCR calibration leads to a model with 11 factors indicating a detection limit of about 3 % foreign fat added. PLS seems to offer the lowest detection-limits (of about 2%) of the methods compared.

In six different ordinary vegetables, namely kohlrabi, Chinese cabbage, chard, leek, spinach and Jerusalem artichoke, zinc was mainly found as low molecular weight species. In the present study, these important zinc compounds are further investigated. The determinations of the metal are performed by ET-AAS. The zinc complexes of all vegetables are anionic at pH 8.0 and show similar elution behaviour in gel permeation and anion exchange chromatography. Consequently, a great resemblance in structure between the low molecular weight zinc species from the different vegetables can be supposed. Exemplary, the zinc complexes of kohlrabi and Chinese cabbage are further examined. In more purified samples of these vegetables compared to zinc neither stoichiometric amounts of free protein amino acids nor nicotianamine, free malic acid, citric acid or phytic acid have been detected. Mainly glutamic acid is found in molar excess to zinc after acid hydrolysis in both cases. The cysteine contents of both zinc-binding fractions are very low. Conclusively, the wellknown γ-glutamylcysteinyl-glycines (phytochelatines) can not be responsible for the bonding of zinc in both ordinary vegetables. We suppose that zinc in kohlrabi and Chinese cabbage is bound to a glutamic acid derivative unknown as yet, possibly a malic acid ester.

The effect of copigmentation of chlorogenic acid with anthocyanins in strawberry and chokeberry juices was investigated. It was found that chlorogenic acid, at concentrations greater than that of anthocyanins, enhanced the colour intensity of these juices. The maximum copigmentation effect in both juices was observed at pH 3.4. In the investigated range of the copigment/pigment ratio, i.e. 1∶1 to 50∶1, absorbance increased (ΔA) linearly with copigment content, ΔA/g chlorogenic acid was greater in chokeberry than in strawberry juices. In solutions of purified pigments of these fruits, smaller copigmentation effects were observed than in juices under the same conditions, which indicates the participation of natural copigments present in fruits in the copigmentation process.

The rheological behaviour of high-fat (22%) and low-fat (8%) meat emulsions during thermal processing in the presence (3%) of various texture-modifying non-meat ingredients, namely maltodextrin, starch, wheat flour, egg white and apple fibre, was analysed. Rheological properties of emulsions were assessed using non-destructive measurements (thermal scanning rigidity monitor, TSRM). The lower the fat content, the lower were the rigidity values of meat emulsions throughout the temperature range studied. Emulsions made with maltodextrin proved less rigid. Addition of starch and egg white favoured the formation of more rigid structures in low-fat meat emulsions at temperatures over 55 °C. Low-fat meat batters containing wheat flour and apple fibre exhibited the highest rigidity values over the given temperature range. The presence of wheat flour caused variations in the modulus of rigidity at all stages of the thermal gelation process, very similar to those observed in high-fat emulsions.

The method of Kwasny for the chemical determination of the organic roasting loss of coffee by analysing trigonelline and niacin has been examined. For this purpose a new gas Chromatographic method for nicotinic acid has been worked out. In contrast to Kwasny, the contents of nicotinamide have not been determined. Data from two roasting series published by Trugo and Macrae have been included. The values for 13 Arabicas of different degrees of roast and of three provenances, as well as five samples of Uganda Robusta correspond fairly well with the results of Kwasny, but two samples of India Robusta do not. Therefore the method of Kwasny seems to be valid in general, but it is necessary to be aware that there are exceptions.

Accurate and reliable data on microgram and nanogram quantities of some essential and toxic elements in most food articles are very scarce. Neutron activation analysis (NAA), with its essentially blankfree advantage, is a valuable approach in the field of determination of trace elements in different foodstuffs and diets. Accordingly, various radiochemical (RNAA) and instrumental (INAA) approaches have been developed in our laboratory for the elements As, Cd, Co, Cu, Hg, I, Mo, Ni, Sb, Se, Sn, Th, U, V, and others, and verified by the analysis of compositionally appropriate certified reference materials.

The giant squid or dosidicus (Dosidicus gigas) is normally shipped frozen from the coasts of America. During the period prior to freezing-when conditions are not always optimum-and during frozen storage, the functional capacity of the muscle proteins declines, rendering the material useless for certain processes such as conversion to gel. This paper examines the reasons for the lack of a good gel-forming capacity as measured both rheologically (breaking force, breaking deformation and gel strength) and in terms of ultrastructure (scanning microscopy). The study was carried out at four different temperatures known to be critical for fish muscle protein gel formation, and at two salt concentrations. At 35°C the structure was spongier in gels made with 1.5% NaCl, although a true gel was still not formed, as shown by rheological measurements. Above 30°C, the ultrastructure became more cellular, particularly in samples made with 2.5% NaCl, at which concentration gel strength values were higher. However, at neither salt concentration nor at any of the experimental temperatures was the mesh as spongy as in other fish gels reported in the literature. The values of rheological analysis and folding test were correspondingly low.

Ten tomato varieties, i.e. Cencara, Daniella, Elena, Ibiza, Lemon Boy, Lucy, Melody, Perfecto, Raf and Rondello, were studied over two consecutive years by GC and GC-sniffing for their differences in flavour composition. Precautions were taken to avoid differences due to the growth conditions and stage of matu-rity. The aroma profiles obtained from dilutions of the extracts confirm the importance of most compounds previously reported as being key flavour compounds in tomatoes. Moreover, they outline a greater number of other key compounds which had not been identified or reported as such in the literature. Among them, 2-methoxyphenol, eugenol, decanal and geranylacetone were identified. Among 39 compounds quantified, 27 were found to permit discrimination between varieties both in 1992 and 1993. Six varieties were characterised in both years by specific flavour compositions. The differences between varieties is due to particular relative amounts of volatile compounds arising from the metabolism of aliphatic amino acids and carotenoids. Volatile compounds arising from each metabolic processes were found to be highly correlated with each other.

Nitrated polycyclic aromatic hydrocarbons (nitro-PAHs) were determined in different kinds of food. The investigation of food matrices necessitates the development of appropriate analytical procedures for sensitive monitoring and determination of these compounds. The analysis of the nitro-PAHs was carried out by GC/MSD, GC plus mass spectrometry, and GC/NPD (nitrogen-phosphorus detection) GC plus nitrogen-phosphorus detection. Seven nitro-PAHs were positively identified and quantified in vegetables, smoked and grilled foods, oils, tea, coffee and spices.

Pumpkin (Cucurbita pepo L.) seed oil is a common salad oil which is produced in Slovenia, Hungary and the southern parts of Austria. It is dark green and has a high content of free fatty acids. The seed itself can be eaten. Due to its colour and the foam formation, the oil cannot be used for cooking. The content of vitamin E, especiallyγ-tocopherol, is very high. The oil content of the pumpkin seed is about 50%. The variability in the oil content is very high resulting from a broad genetic diversity. Thus a breeding programme for increasing the oil productivity is very promising. The four dominant fatty acids are palmitic, stearic, oleic and linoleic acids. These four fatty acids make up 98±0.13% of the total amount of fatty acids, others being found at levels well below 0.5%.

Liquid chromatography has been used as a means of egg protein analysis or as a method for the purification of egg proteins. Several Chromatographic methods, including gel permeation, ion-exchange, reversed-phase, hydrophobic interaction, and immobilized-ligand-affinity chromatography, have been carried out for the separation or the purification of egg yolk or egg white proteins. Ion-exchange chromatography appears to be the most frequently used method for protein isolation and it is the easiest to adapt to a process scale. From an analytical point of view reversed-phase chromatography is, at the moment, the recommended method for egg white analysis. Egg white has been fractionated more often by liquid chromatography than has egg yolk. Several Chromatographic methods have been developed on a laboratory scale, but the application of these techniques on an industrial scale remains limited.

To investigate amino acid changes in green coffee beans in the post-harvest period, amino acid concentrations were determined in green beans and after modelled drying, fermentation and storage. After the drying at alternating temperatures up to maximally 40°C, considerable changes in the concentrations of individual amino acids were identified. At the beginning of the storage period, significant changes in concentration were found to a minor extent. Under the condition of drying, it was mainly the concentration of glutamic acid that changed considerably. There was an increase in all the samples by 500 mg/kg dry matter on average, which corresponds to an increase of about 50% of the original value. In contrast, the concentration of aspartic acid in most of the samples decreased clearly due to drying. For the predominant part of the coffee samples, there was a significant increase in the hydrophobic amino acids Val, Phe, Ile and Leu. Changes of the quantities of other amino acids were non-uniform and only insignificant. Constant drying at 80°C for most of the amino acids brought about only minor concentration changes compared to those values obtained at 40°C. Modelled fermentation had no significant effect on the concentrations of the individual amino acids. After a 4-week storage of dried beans, amino acid concentrations did not change further. It is very possible that different post-harvest treatment parameters may influence the amount of aroma precursor compounds in the coffee beans.

An indirect competitive enzyme-linked immunosorbent assay (ELISA) has been developed for the detection of native and heat-denatured bovineβ-lactoglobulin (hd-β-lg) in goats' and ewes' milk cheese. Polyclonal antibodies raised in chicken against hd-β-lg were purified by immunadsorption chromatography on native bovine, ovine and caprineβ-lactoglobulins conjugated to CNBr-activated Sepharose. Although lactoglobulins from ewe, goat and cow have very similar amino acid sequences, crossreactivity was eliminated completely by this procedure. A commercially available goat-anti-chicken alkaline phosphatase conjugate was used as a secondary antibody to detect the anti-hd-β-lg antibodies bound to immobilized hd-β-lg. The detection limit of the assay was 100 ng/ml bovine native lg or hd-β-lg or 0.1–0.2% of cows' milk equivalent in cheese. Within a method validation study of the European Union, the ELISA test was successfully applied for the detection of native and heat-denatured bovine whey proteins in ewes' and goats' milk cheeses.

On-line supercritical CO₂ extraction - gas chromatography was applied to the isolation and identification of free fatty acids and other volatile compounds of young and ripe Swiss cheese (Emmental) produced in Finland. Extractions were carried out using a micro-cartridge at 40 °C temperature and 10 MPa pressure and the volatile fractions were analysed by DB-WAX column (polyethylene glycol phase) with flame ionization detection and mass spectrometry. The total time of analysis was less than 2.5 h. Acetic acid and propionic acid predominated over the C12–C18 acids, the longer chain fatty acids increasing in concentration during the ripening of the cheese. Due to the high proportions of fatty acids, further fractionation is required for analysis of the less abundant aroma compounds such as alcohols, carbonyls and lactones.

Flavour models were developed for two samples (A and B) of Swiss cheese which differed in their ripening stage and flavour profile. The models were based on an unripened, freeze-dried cheese of the Mozzarella type. Compounds which, in previous studies had been screened as contributors to the odour and taste of Swiss cheese, were added to the base in various combinations and at concentrations equal to those found in Swiss cheeses A and B. Models composed of methional, 4-hydroxy-2,5-dimethyl-3(2H)-furanone, 2-ethyl-4-hydroxy-5-methyl-3(2H)-furanone, acetic acid, propionic acid, lactic acid, succinic acid, glutamic acid, sodium, potassium, calcium, magnesium, ammonium, phosphate and chloride were judged to meet the flavour of Swiss cheese very well.

Adulteration of expensive edible oils, such as olive oil, often involves desterolized oils in order to render the adulteration undetectable. Sunflower oil contains characteristic Δ7-sterols, which are readily removed upon strong bleaching. It is shown that these Δ7-sterols do not primarily dehydrate (as do Δ5-sterols), but isomerize to Δ8(14)- and Δ14-sterols. These compounds can be analysed by LC on silica gel or GC on capillary columns with stationary phases of intermediate to high polarity.

An HPLC study of the carotenoid composition of fresh, frozen and canned papaya fruit slices was done. There were no qualitative differences between the carotenoid patterns of fresh and frozen papaya fruit slices (cultivar Sunrise). The major carotenoids found in papaya extracts were lycopene and carotenol fatty acid esters ofβ-cryptoxanthin andβ-cryptoxanthin-5, 6-epoxide. Other xanthophylls detected wereβ-crypto-xanthin,trans-zeaxanthin and cryptoflavin. It was possible to determine the quantitative losses of carotenoids in papaya slices as a result of the freezing process and frozen storage, since samples of these fruits were available before processing. The pigment pattern of the canned product showed lycopene as being a major pigment. Thermal treatment induced the degradation of carotenol fatty acid esters of xanthophylls. The freezing and canning processing of papaya slices led to significant decreases in the total carotenoids quantified by HPLC, with frozen female slices and canned samples showing lower amounts of pigments. Hunter colour values of frozen slices were similar to those of fresh papaya fruit slices.

This study determines ash, K, Ca, Na, Mg, Fe, Cu, Pb, and Zn content in musts and wines of the DOC Tacoronte-Acentejo (Tenerife, Canary Islands) from two consecutive harvests. Samples were treated with HNO₃ and H₂O₂. Na and K were determined by flame photometry and the remaining metals by air/acetilene flame atomic absorption spectrophotometry. Significant differences were observed in Na, Ca and Mg contents between both harvests, possibly due to climate conditions.

Capsaicin, dihydrocapsaicin and nordihydrocapsaicin were determined in paprika powders and oleoresins after clean-up on silica and aluminium oxide with controlled activity followed by isocratic reverse-phase HPLC (RP-HPLC) with fluorescence detection. Caprylic acid vanillylamide (CVA) was synthesized for use as internal standard. Samples with less than 0.6 μg/g (10 Scoville Heat Units) were analysed.

Daily dietary chromium intake in Belgium has been evaluated by sampling duplicate portions of food, heating them at an acidic pH in a microwave oven and then quantifying the chromium by atomic absorption spectrometry. The mean intake value (53±31 μg/day) is similar to levels found for most other countries and is situated at the lower end of the recommended range for a safe and adequate daily dietary intake.

Two cultivars of chickpeas (Cicer arietinum) and one cultivar of lentils (Lens culinaris) were subjected to germination in the dark for 6 days at 20°C. Soyasaponin VI, also known as soyasaponinβg, a DDMP- (2,3-dihydro-2,5-dihydroxy-6-methyl-4H-pyran-4-one-) conjugated form of soyasaponin I, was the only saponin detected in both the unprocessed and germinated seed. No significant changes in saponin content were observed for chickpeas or lentils after a 6-day germination.

The detection of adulteration of wine by SNIF-NMR (site-specific natural isotopic fractionation-nuclear magnetic resonance) analysis of wine alcohol is a well established and widely used method. Quantitative deuterium ([²H]) NMR spectroscopy of defined distillate/tetramethylurea (TMU) mixtures enables the calculation of the site-specific deuterium/hydrogen ([²H]/H) ratios in the ethanol molecule. TMU with a known [²H]/H ratio serves as the internal standard. The comparison of the [²H]/H ratios of unknown samples with values obtained from authentic samples allows conclusions to be drawn, in terms of the origin of the sugar in the must before fermentation. Up to now, the calculation of [²H]/H ratios has required the exact weighing of both the distillate and the quantity of TMU for the tube preparation, as they affect²H-NMR measurements. The precise quantity of ethanol in the distillates must be determined by Karl-Fischer titration or densitometry. Volatile distillate components are quantified by gas chromatography to ensure a satisfactory purity of the ethanol under study. The quantitative¹H-NMR method described involves determining the TMU/ethanol mass ratios in the tubes prepared for SNIF-NMR measurements. This mass ratio is necessary for the calculation of the [²H]/H ratio. The mass ratios measured using conventional procedures and those determined by on-line¹H-NMR agree 100%. Using this method means that the exact weighing of distillates and TMU for tube preparation and the determination of ethanol content in the distillates are no longer required. At the same time, higher concentrations of volatile components in the distillates, e.g. methanol, can be easily detected.

Influence of saliva composition and volume on flavour release from rehydrated French beans (Phaseolus vulgaris) was studied in three types of mouth model systems; dynamic headspace (DH), dynamic headspace and mastication (DHM) and a purge-and-trap (PT) model system. Volatile compounds were analysed by gas chromatography, using flame ionization detection (FID), mass spectrometry and sniffing port detection. Areas of FID peaks were largest in the PT system, followed by those of the DHM and DH systems, respectively. Saliva composition as well as volume influenced the release of volatile compounds from rehydrated French beans. Generally, FID data showed a decrease in release by the saliva component mucin, because of interactions between volatile compounds and protein, and an increase in release by its α-amylase, probably due to degradation of inclusion complexes of starch. The decrease in flavour release by the enlarged saliva volume was evaluated by a model study. Sniffing patterns of odour active compounds were barely influenced by either saliva composition or volume.

A comparative study was made of the influence of freezing (−24°C) and frozen storage (−12°C) on the functional properties (viscosity, solubility) and physico-chemical characteristics (aliphatic and aromatic hydrophobicity, ATPase activity) of actomyosin (AM) from myosystems (chicken and hake) of differing freezing and frozen stability. The difference in functional behaviour between chicken and hake AM as a consequence of freezing and frozen storage suggests that, for hake AM, denaturation and aggregation occur essentially through direct aggregation of AM molecules to produce AM aggregates, whereas in chicken proteins, AM first dissociates into myosin and actin to produce myosin and myosin-actin aggregates.

The direct enantioseparation of 2-phenylpropanol, 2-phenylpropanal and 2-phenylpropanal dimethyl acetal was achieved, using enantioselective gas chromatography and heptakis-[2,3-di-0-acetyl-6-0-tert.butyldimethylsilyl]-β-cyclodextrin (DIAC-β-CD) or octakis-[2,3-di-0-acetyl-6-0-tert.butyldimethylsilyl]-γ-cyclodex-trin (DIAC-γ-CD) as the chiral stationary phase. Their odour characteristics and threshold values were investigated by enantioselective gas chromatography/olfactometry. Starting from commercially available (R)-2-phenylpropionic acid, enantiopure (R)-configured reference compounds were synthesized.

In diethyl ether extracts from celeriac (Apium graveolens L. var.rapaceum) all four stereoisomers of (3a–7a)-cis-3-butylhexahydrophthalide were found to be present. The analyses were carried out by means of GC, enantioselective GC and GC-MS. The assignment of the relative configuration of the diastereomers3 and4 was accomplished by NOE difference spectroscopy.

The ability of fermentative CO₂ to blow off the volatile compounds that are synthesized during fermentation has been studied. Model solutions simulating a fermenting must were purged at different CO₂ flow rates and temperatures, and the amount of volatile compounds blown off by the stream of CO₂ was recorded by high-resolution gas chromatography. Data showed that under normal fermenting conditions, fatty acid ethyl esters and some fusel alcohol acetates are blown off the solution at a high rate. The maximum loss rate was observed for ethyl decanoate. The purging speed is doubled when temperature increases from 17 °C to 27 °C. Losses can be interpreted by a linear model and are a function of the compound and the flow rate of CO₂. These models allow us to reconstruct the volatile synthesis vs time functions through graphic calculus and to estimate the proportion of volatile material retained, hydrolysed and purged. Synthesis takes place during the tumultuous period of fermentation together with CO₂ production that blows off the volatile material. Hydrolysis takes place in the last stages of fermentation. In a 10-1 open fermenter, up to 80% of volatile material can be blown off while an average of 10% is retained. Residual esterase activity accounts for about 20% of the total amount of ester synthesized.

A new method for the specific and sensitive detection of soya (Glycine max) in processed meat products has been developed using polymerase chain reaction (PCR) technology. The presence of soya deoxyribonucleic acid (DNA) from several soya protein concentrates was determined with two pairs of specific oligonucleotides yielding a 414-bp (bp=base pair) fragment and an internal 118-bp fragment amplified from the soya lectinLe1 gene. The test detected DNA from textured soya protein concentrates in meat products at a level of 1% and was confirmed by a commercially available enzyme-linked immunosorbent assay (ELISA).

Soluble and isoelectric soluble soybean protein hydrolysates were prepared by Alcalase treatment to a degree of hydrolysis of 3–15%. The bitterness intensity of the hydrolysates obtained was assessed on a five-point scale. The average relative molecular masses of peptides in the soluble hydrolysates (2250-1400) and isoelectric soluble hydrolysates (1313-800) and their hydrophobic peptide fractions (575-400) were determined by the trinitrobenzenesulphonic acid method. The molecular mass distribution of peptides in soluble and isoelectric soluble soybean hydrolysates and their hydrophobic peptide fractions was determined by gel permeation HPLC using a Zorbax Bio Series GF-250 column. The results suggest that the main reason for the bitterness of soybean protein hydrolysates prepared by Alcalase treatment are hydrophobic bitter peptides of relative molecular mass less than 1000.

Chicken breast was irradiated with doses of 3, 5, and 7 kGy. Headspace gas chromatographical analysis demonstrated the tendency that the amounts of volatile compounds (mainly pentanal, hexanal and heptanal) are higher in irradiated samples in comparison with non irradiated. Statistical evaluation of the gas chromatograms by discriminant analysis enabled the detection of irradiation. Unknown samples could be classified in the groups „unirradiated“ or „irradiated in most cases.

Botryodiplodia theobromae, Rhizopus oryzae, Aspergillus niger, A. flavus and Fusarium equiseti were found to be associated with the ripening of bananas and also caused rot during storage. Bananas stored in baskets with ash fire wood ripened 2–3 days earlier than bananas stored in fibre sacks and under constant light. The infected bananas showed a decrease in the quantity of total soluble sugars, protein, lipid, crude fibre, ash, ascorbic acid and mineral elements when compared with the control fruit. Paper Chromatographic studies showed the presence of glucose, sucrose, fructose, maltose and raffinose in healthy control fruit, while only sucrose appeared during storage in bananas infected withB. theobromae. The total soluble sugar and crude protein contents increased during ripening.

A method for quantitative isolation of melanoidins (coloured polymer compounds) from beer has been developed. It shows good reproducibility with respect to the results with a relative error of less than 7%. Physical and spectral methods were used to characterize the melanoidins. They were subjected to thermal treatment under model conditions. The volatile destruction products, half of which known as flavour components, were isolated. This allows the authors to classify melanoidins as participants in the flavour-forming processes in beer.

Growth, substrates and end-product formation of the maltose and citrate co-metabolization byLactobacillus brevis subsp.lindneri CB1 citrate-negative strain were initially studied in synthetic medium. Compared to maltose (19 g/l) fermentation, the co-metabolization of maltose (10 g/l) plus citrate (9 g/l) caused faster cell growth, increased the concentrations of lactic acid and especially of acetic acid (from 0.7 g/l to 2.9 g/l), produced succinic acid (0.5 g/l) and reduced ethanol synthesis. Highest activities of acetate kinase, the same of lactate dehydrogenase and a reduced alcohol dehydrogenase activity were detected in cytoplasmic extracts of cells growing on maltose plus citrate. The breakdown of citrate depended upon the continuous presence of maltose in the growth medium. Upon depletion of citrate, the cells continued through the normal maltose fermentation, having a diauxic metabolic curve as shown by impedance measurements. Concentrations of citrate from 3 g/l to 15 g/l led to increases of acetic acid from 1.25 g/l to 5.55 g/l. Since maltose was naturally present during sourdough fermentation, the addition of 9 g citrate per kg wheat dough enabled the co-metabolization of maltose and citrate byL. brevis subsp.lindneri CB1. Compared with traditional sourdough fermentation, faster cell growth, a higher acetic acid concentration and a reduced quotient of fermentation were obtained by co-metabolism.

In the present work we discuss the usefulness of carbon isotope analysis of wine ethanol for the assignment of origin and the proof of adulteration of Italian, French and German wines. At first the comparability of the results from three laboratories is demonstrated by the results of inter-laboratory comparison measurement and by tests of the distillation procedures applied to the same samples. Furthermore, a close correlation of carbon isotope content in sugars from must and ethanol from the related wine could be found for samples from all countries. Using the δ¹³C values of EC data bank wines from 1991 to 1993 for Italy, France and Germany, we describe and discuss the main factors of influence which are responsible for the variation of those values. By examination of spiked samples, the usefulness of the δ¹³C analysis in the detection of certain types of wine enrichment is demonstrated; especially if the carbon isotope analysis by¹³C-8 isotope ratio mass spectrometry is employed as an additional tool for improving the security of the already officially performed determination of the site-specific hydrogen isotope content in wine ethanol by²H-NMR.

A recently designed system of steam distillation solvent extraction (SDE) was applied to the preparation of samples for GC analysis of volatile components in heat-treated milk. In order to evaluate the effect of the SDE sample temperature on the original composition of the milk, model systems with different sensitivities to heat were submitted to the SDE process at normal pressure. Finally, the usefulness of the method for the differentiation of heat-treated milk samples was evaluated.

The quality of an α-tocopherol standard can be checked easily by measuring the UV absorbance at minimum (255 nm,A_min) and maximum (292 nm,A_max) wavelengths inn-hexane. If the quotientA_min/A_max exceeds 0.18, the standard contains less than 90% α-tocopherol and the determination at 292 nm will yield inaccurate results.

Apple pulp suspensions to which different kinds of pectin in concentration up to 500 g.m⁻³ was added were studied electrophoretically. It was shown that the natural pectin exerts an essential influence upon the adsorption ability of the pectin added, and upon the electrokinetic potential of the tissue particles respectively.

Changes in free reduced glutathione (GSH), free oxidised glutathione (GSSG) and protein-glutathione mixed disulphides (PSSG) during dough mixing were monitored. After a rapid decrease in the GSH content and an increase in the GSSG content, the contents of both GSH and GSSG decreased progressively, whereas the PSSG content increased, as a simple flour-water dough was mixed. Total glutathione (GSH plus GSSG plus PSSG) levels in simple flour-water doughs and doughs treated with ascorbic acid or potassium bromate remained essentially constant during dough mixing, indicating that the reactions in which glutathione is involved are simple oxidations of sulphydryl (SH) groups to disulphide (SS) bonds and SH/SS interchange reactions. Yeast contributed high levels of GSH and GSSG to doughs, but analysis of dough aqueous phases (liquors) and the similarity of the PSSG contents of simple and yeasted flour-water doughs suggested that the yeast GSH and GSSG were largely unavailable to react with flour proteins. The GSH content of ascorbic-acid-treated and yeasted dough decreased rapidly on wetting the flour, the magnitude of the decrease indicating that the ascorbate oxidation system oxidised the yeast intracellular GSH as well as the flour GSH. With further mixing, the GSH content of the ascorbate dough remained constant at low levels similar to those of the simple flour-water dough. The GSSG content of the ascorbate dough increased rapidly on wetting the flour, but declined as dough mixing continued. The PSSG content of the doughs increased markedly as dough mixing proceeded to the optimum and then stabilised. The increase in the PSSG content lagged behind the rapid oxidation of GSH to GSSG. Potassium bromate caused a pattern of changes similar to those observed for ascorbate, but the changes in GSH and PSSG contents were smaller in magnitude. The results indicate that the changes in the different glutathione pools and the effects of oxidising bread improvers are rather more complex than envisaged previously, particularly the effects on PSSG.

This paper describes the application of thermospray-HPLC-MS (buffer ionization mode, single-stage MS, positive ion detection) to the analysis of flavanols (catechins), flavonolO-glycosides, flavoneC-glycosides as well as caffeine, theobromine, theogallin and theanine from tea. All compounds are detected as pseudo-molecular ions [M+H]⁺. Other molecular ion species are adducts with sodium, potassium, ammonium and solvent clusters. The catechin gallates and the flavonol glycosides are fragmented. The fragmentation is temperature dependent. The glycoside bond is labile and consequently the flavonol glycosides have the protonated aglycone as this base peak. The ester bonds in the catechin gallates are more stable and the fragmentation is limited. The fragment pattern contributes to the structural information. LC-ther-mospray-MS is a good analytical tool for identifying the polyphenols mentioned above both in tea and other foodstuffs, especially in method development and structural elucidation.

To detect those fruits which have been subjected to low-dose irradiation (0.5-3 kGy), two methods of chromatography (GC-MS and LC-LC-GC-FID) were used to determine the radiolytic compounds of lipids formed after irradiation, such as alkanes and alkenes. Extraction of volatile hydrocarbon compounds from some parts of irradiated fruits, e. g. the flesh (avocado), seeds (papaya) and kernels (mango and apricot) was carried out. The analysis of hydrocarbons by GC-MS proved the suitability of using C17∶1, C16∶2, C15∶0 and C14∶1 as markers for avocados irradiated with a low dose (0.75 kGy). The same indicators appeared following the analysis of papayas and mangoes irradiated with 1.5, and 3.0 kGy. Also, C15∶0, C14∶1 and C16∶3 can be used to identify apricots irradiated with a low dose (0.5 kGy). The detection of alkenes was only improved by a more selective isolation, e.g. of dienes or trienes by LC-LC-GC-FID. Within a few minutes, apricots and avocados irradiated at low doses (0.5 and 0.75 kGy) can be recognized by the indicators C16∶2, C17∶2 and C16∶3, without interfering peaks. In all cases, C16∶1, C16∶2, C16∶3 as well as significant amounts of C17∶2 can be used as markers for fruit irradiation.

This paper seeks to compare the ultrastructure of gels made from frozen muscle of giant squid (Dosidicus gigas) at various temperatures with a number of different rheological parameters, with reference to a variety of added ingredients (non-muscle proteins and hydrocolloids) and to NaCl concentration. Interesting data on gel rheological properties were found where formulae containedl-carrageenan, starch and egg white, with a low salt concentration (1.5%). This seems to be because carrageenan forms an independent network which supports the principal structure formed by the fish protein; starch is incorporated into the network and retains water; and egg white forms a supplementary network which helps to improve rheological properties.