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1.
A gas chromatographic (GC) method has been developed for the simultaneous quantitation of fatty acids and sterols in orange juice, using a bonded phase fused silica capillary column of intermediate polarity, splitless automatic injection, and flame ionization detection. Sample preparation has been simplified by using 1 g C-18 adsorbent in a disposable minicolumn to extract 2 mL orange juice. Methylation of fatty acids and silylation of the sterols were carried out in the eluted extract (low polarity lipid fraction). The method precision was 7%; recoveries ranged from 83 to 113%. The precision of the injection technique was 2%. Seven major fatty acids and 5 sterols in orange juice were quantitated by the GC method and identified by GC/mass spectrometry. Quantitative data for several orange juice samples indicated that the levels of the compounds of interest were in the 1.3-72.0 mg/L range. The results demonstrate that bonded phase fused silica capillary GC has great versatility and potential for the quantitative determination of fatty acids and sterols.  相似文献   

2.
The contents of potentially toxic elements lead and cadmium and the essential element copper in various milk and dairy products consumed in Turkey were determined by differential pulse polarography (DPP), primarily to assess whether the intakes comply with recommended desired concentrations for essential and permissible levels for toxic elements. A simple and rapid DPP method has been developed for the simultaneous determination of cadmium, lead, and copper in samples. Using the differential pulse mode, half-wave peak potentials as E(1/2) were -0.58, -0.40, and -0.07 V for cadmium (Cd), lead (Pb), and copper (Cu), respectively. Marketed formulations of dairy products have been analyzed by calibration and standard addition methods. Recovery experiments were found to be quantitative. The linear domain ranges were 0.00-674.28 microg/L for Cd (R2 = 0.9999), 0.19-2.94 mg/L (p < 0.01) for Pb (R2 = 0.9997), and 0.41-133.46 microg/L for Cu (p < 0.01) (R2 = 0.9999). The studies have shown that the method is a rapid, reproducible, and accurate determination of these elements in milk and dairy products and can be used in the analysis of marketed formulations in the milk and dairy industry.  相似文献   

3.
An isocratic liquid chromatographic (LC) technique is described for the determination of benzoic acid and sorbic acid in foods such as beverages, fruits, seafood, vegetables, sauces, and dairy, bakery, and confectionery products. A C18 column is used with methanol-phosphate buffer (5 + 95) as mobile phase and 4-hydroxyacetanilide or 3,5-dinitrobenzoic acid as internal standard. Sample preparation is simple, rapid, and produces a sample extract that has a minimum effect on the column performance and life. Specificity of the method was checked against common food additives such as L-ascorbic acid, caffeine, artificial sweeteners (saccharin, cyclamate, aspartame), antioxidants (BHT, BHA) and artificial colors. Also described are 2 procedures for confirmation of the preservatives, using either redox reaction of sorbic acid with potassium permanganate or gas chromatography/mass spectrometry. Mean recoveries of 90-105% were obtained with a precision of 1-6% and a detection limit of 20 mg/kg for the 2 preservatives.  相似文献   

4.
Furosine: a suitable marker for assessing the freshness of royal jelly   总被引：7，自引：0，他引：7  
Fifteen commercial samples of royal jelly, consisting of 10 imported samples, and 5 samples of known origin obtained freshly harvested from beekeepers, were analyzed for protein, lysine, and furosine content. In addition, a commercial sample of royal jelly, at the beginning of its commercial shelf life, was stored for 10 months both at 4 degrees C and at room temperature in order to assess the development of the Maillard reaction (furosine) and relative nutritional damage (blocked lysine). The commercial royal jelly products contained different amounts of furosine, ranging from 37.1 to 113.3 mg/100 g protein, evidence of different storage times and conditions. The average furosine content of the royal jelly samples of known origin and harvesting was significantly lower than that of the imported samples (41.7 versus 73.6 mg/100 g protein, respectively). With regard to shelf life, furosine content increased significantly from 72.0 mg/100 g protein to 500.8 mg/100 g protein after 10 months of storage at room temperature, while it increased to a much lower level (100.5 mg/100 g protein) when the royal jelly was stored at 4 degrees C. However, nutritional damage, expressed as blocked lysine (calculated indirectly from the furosine content), was minor or negligible, 11.9 and 2.3% of total lysine, in samples stored at room temperature and at 4 degrees C, respectively. Lysine was determined by an innovative procedure based on high-performance anion-exchange chromatography with pulsed amperometric detection (HPAEC-PAD). The results showed that furosine is a suitable index for assessing the quality and freshness of royal jelly.  相似文献   

5.
Browning indicators in bread   总被引：7，自引：0，他引：7  
Bread is the most important food in the Spanish household and represents the largest proportion of products produced by commercial bakeries. The browning indicators furosine, hydroxymethylfurfural (HMF), and color were determined to evaluate heat effects induced during manufacture of these foods. The breads analyzed were common, special, sliced toasted, and snack breads. Identical sample preparation and HPLC conditions were used to determine HMF in all breads. The precision tested at high and low HMF concentration in breads was 2.60% and 1.57%, respectively. Recovery of HMF was 96.2%. The HMF values ranged from 2.2 to 68.8 mg/kg. Color index (100 - L) ranged from 17.0 to 38.2. The linear correlations (r(2)) between 100 - L/HMF were above 0.70 for common, special, and snack breads. Similar correlation was obtained between 100 - L/HMF in a dough baking at different times. The furosine content in common bread ranged between 125 and 208 mg/100 g of protein. No linear correlation was found between furosine and HMF. Moreover, HMF and furosine were also determined in crumb and crust. Levels of HMF had a wide range (0.9-1.76 mg/kg) and furosine was between 43 and 221 mg/100 g of protein.  相似文献   

6.
The effect of freeze-drying and the assessment of the storage stability of freeze-dried royal jelly (RJ) were investigated by the determination of furosine and blocked lysine. The level of furosine in the RJ samples collected from cells at different times (1, 2, and 3 days after grafting) showed that the Maillard reaction had already occurred in the hive as indicated by the increase in furosine: from 9.6 to 20.8 mg/100 g of protein. Freeze-dried RJ was more prone to the early stage of the Maillard reaction than fresh RJ, as confirmed by the significantly higher furosine values found after 12 months, both at 4 degrees C (253.4 versus 54.9 mg/100 g of protein) and at room temperature (884.3 versus 332.5 mg/100 g of protein). After 18 months at room temperature, the lyophilized samples reached a furosine level of 1440.4 mg/100 g of protein, which corresponded to the blocked lysine levels, amounting to 24% of total lysine.  相似文献   

7.
In this work, the quantitation of cellular carbohydrates, namely chitin and glucan, in peanut fungal pathogens and baker's yeast was carried out by capillary electrophoresis (CE) and capillary electrochromatography (CEC). The chitin and glucan of the fungi were hydrolyzed by the enzymes chitinase and glucanase, respectively, to their corresponding sugar monomers N-acetylglucosamine (GlcNAc) and glucose (Glc). These two monosaccharides were then tagged with 6-aminoquinoline (6-AQ) to allow their separation and detection in CE and CEC. The 6-AQ derivatives of GlcNAc and Glc formed the basis for the determination by CE and CEC of chitin and glucan in peanut fungi and baker's yeast. Several parameters affecting the separation of the 6-AQ derivatives of GlcNAc and Glc, including the separation voltage and the composition of the running electrolyte, were investigated. Under the optimized separation conditions, the contents of cellular carbohydrates including N-acetylglucosamine, chitin, glucose, and glucan in some fungi, such as Sclerotinia minor, Sclerotium rolfsii, and baker's yeast, were successfully determined. The method described here allowed the assessment of genetic differences in Sclerotium rolfsii isolates from various locations.  相似文献   

8.
The extent of the Maillard reaction was studied by measuring furosine and color formation in infant and enteral formula-resembling model systems prepared by mixing calcium caseinate, laboratory-obtained or commercial whey protein with lactose or dextrinomaltose (ingredients similar to those used in infant and enteral formula manufacture) and heating the mixture at 100, 120, or 140 degrees C for 0-30 min. The furosine determination was performed by HPLC and the color determination by measuring colorimetric parameters L, a, and b in a reflection photometer. The first steps of the Maillard reaction could be followed by furosine determination when initial ingredients had low thermal damage. Hence, furosine may be an indicator of low thermal damage in ingredients with <100 mg/100 g of protein. At the concentrations used in these model systems, similar to those in infant and enteral formulas, furosine values (indirect measure of lysine losses) were higher in lactose than in dextrinomaltose systems, in which only glucose, maltose, maltotriose, and maltotetraose among all of the sugars present showed reactivity with casein. Finally, the advanced steps could be followed by color determination when the initial ingredients had high thermal damage or the model systems were heated at high temperature or for a long time. Among the parameters assayed, b was the most sensitive.  相似文献   

9.
A capillary electrophoresis (CE) method was developed for the profiling and determination of individual glucosinolates (GSs) via their isothiocyanate degradation products upon myrosinase digestion. The resulting isothiocyanates, the structures of which are reflective of the parent GS's, were then converted to their corresponding amines via base hydrolysis or reaction with 1, 2-benzenedithiol. Subsequently, the amines were fluorescently labeled to allow their sensitive detection by laser-induced fluorescence (LIF). The CE method involved the use of in situ charged micelles for the separation of isothiocyanates and their corresponding fluorescently labeled amines by micellar electrokinetic capillary chromatography (MECC). The term "in situ charged micelles" refers to micelles formed by complexing the polar hydroxyl groups of glycosidic surfactants with borate. The MECC method with on-column LIF detection was applied to the determination of GSs in white cabbage, rapeseed leaves, and rapeseed roots.  相似文献   

10.
A gas chromatography-mass spectrometry (GC-MS) method was used for the quantitative confirmation of phosphine residues in stored products and processed foods. An established extraction technique was utilized for the preparation of headspace samples, which were analyzed by GC-MS and gas chromatography-nitrogen-phosphorus detection (GC-NPD). Wheat, oats, maize, white rice, brown rice, cornflakes, tortilla cornchips, groundnuts, and raisins were validated, showing excellent agreement between detectors when spiked at levels equivalent to 0.001 and 0.01 mg/kg phosphine and for samples containing incurred residues. The GC-MS method was reproducible and accurate when compared to the GC-NPD method and allowed five samples to be quantified in a working day. Subambient GC-MS oven temperatures were most suitable for phosphine residues ranging from 0.001 to 0.005 mg/kg, and a GC oven temperature of 100 degrees C was appropriate for residues >0.005 mg/kg. The method was sufficiently robust to be evaluated for other similar commodities as the need arises.  相似文献   

11.
The reaction kinetics of two heat damage indices, HMF and furosine, were examined in four tomato products with different dry matter contents (10.2, 25.5, 28.6, and 34.5%) over a temperature-time range of 80-120 degrees C and 0-255 min. The reactions followed pseudo-zero order kinetics. E(a) and z-value were, respectively, 139. 9 kJ/mol and 19.2 degrees C for HMF, and 93.9 kJ/mol and 28.4 degrees C for furosine. The analyses of both indices in several samples of commercial and industrial tomato products showed very low levels of HMF (from 1 to 42 ppm) and a lack of correlation between HMF and furosine mainly because of the different evolution of the two indices during storage. The HMF level of a tomato paste sample stored at 25 degrees C decreased from 609 to 17 ppm after 98 days, while furosine increased from 458 to 550 mg/100 g of protein.  相似文献   

12.
For nutritional purposes the recombination of milk or milk proteins with polyunsaturated fatty acids had long been considered in newly designed products, such as functional foods. Four milk-resembling model systems were prepared having malondialdehyde content ups to 1 mM. Systems were heated between 110 and 150 degrees C for up to 30 min. The effect of the presence of bifunctional aldehydes on the determination of furosine as a heat-induced marker was investigated. Levels of 0.01 mM MAD in the reaction mixture could affect significantly the determination of furosine in a milk-based system. Impairment of lysyl residues through the analysis of furosine could be underestimated in the presence of malondialdehyde.  相似文献   

13.
A reverse-phase liquid chromatographic method is described for the determination of carminic acid in yogurt. A C18 column is used with acetonitrile-1.19M formic acid (19 + 81) as mobile phase and diode array detection. Sample preparation includes deproteinization with papain and purification in a polyamide column. The relative standard deviation for repeated determinations of carminic acid in a commercial strawberry-flavored yogurt was 3.0%. Recoveries of carminic acid added to a natural-flavored yogurt ranged from 87.2 to 95.3% with a mean of 90.2%. The method permits measurement of amounts as low as 0.10 mg/kg.  相似文献   

14.
A micellar electrokinetic capillary chromatography (MECC) mode was applied to a capillary electrophoresis (CE) method, which was developed for detection and quantitation of patulin in apple ciders. This method used a small sample amount (2 mL) and consumed minimal organic solvent compared to the most commonly used HPLC methods. The sample preparation procedure of the CE method was also simpler than other chromatographic techniques developed for patulin analysis. Patulin was detected with a photodiode array detector at 273 nm. The standard curve was linear (r(2) = 0.9984) from 75 microgram/L to 121 microgram/mL with patulin working solutions corresponding to 3.8 microgram/L to 6.1 microgram/mL patulin in the sample. The linearity was better in a narrower range of concentrations (r(2) = 0.9999) from 75 microgram/L to 24.1 microgram/mL. The limit of detection of the method was 3.8 microgram/L. Patulin recoveries at 4 levels in spiked samples (10-121 microgram/L) ranged from 95.2 to 105.4%. The recoveries were 96. 9% and 99.2% for 2 levels (22.3 and 223 microgram/L, respectively) of patulin in infected apple samples. This method represents a unique alternative method for rapid and sensitive analysis of patulin in apple ciders.  相似文献   

15.
Solid phase microextraction (SPME) and gas chromatography were used for tequila volatile characterization and ethyl ester quantitation. Several factors determined the differences in tequila volatile profiles obtained by the SPME technique, namely, sampling mode, fiber coating, and fiber exposure time. Each of these factors determined the most suitable conditions for the analysis of volatile profiles in tequila. Volatile extraction consisted of placing 40 mL of tequila in a sealed vial kept at 40 degrees C. A poly(dimethylsiloxane) fiber was immersed in the liquid for 60 min and desorbed for 5 min into the gas chromatograph. The identified volatiles by mass spectrometry were mainly alcohols, esters, and ketones. The calibration curves for ethyl hexanoate, octanoate, and decanoate followed linear relationships with highly significant (p < 0.001) determination coefficients (R2 = 0.99). The coefficients of variation of less than 10% for ethyl ester concentrations indicated that the technique was reproducible. The limits of quantitation for ethyl esters were 0.05 parts per million, which were below the concentration range (0.27-15.03 ppm) found for different tequila samples. Quantitative differences in ethyl esters were found for the four most commonly known tequila types: silver, gold, aged, and extra-aged.  相似文献   

16.
Results of pesticide and industrial chemical residue determinations, using both capillary and packed column gas chromatography (GC), in 3 Food and Drug Administration (FDA) laboratories have been compiled and compared. Samples consisted of food products collected for routine residue screening by the respective laboratories. Extracts were prepared by conventional multiresidue methodology. Capillary column systems and operating conditions were selected at the discretion of each laboratory and were therefore variable, although split/splitless injectors in the split mode were used with prescribed precautions in all cases. Packed column systems were operated as specified in the FDA Pesticide Analytical Manual (PAM). Overall correlation between the 2 systems, expressed as the average ratio of packed column result to capillary column result, was 0.99 for 120 determinations in 41 samples. The higher resolving power of the capillary systems allowed quantitation of several residues that were incompletely separated and therefore unquantifiable using the packed columns. Capillary column GC with the split injection technique, used with appropriate precautions, was found to be both reliable and advantageous for regulatory determination of pesticide and industrial chemical residues in foods and feeds.  相似文献   

17.
Organic acids are relevant in dairy products for nutritional reasons and because they contribute to the flavor and aroma. They are the major products of carbohydrate catabolism of lactic acid bacteria and nonstarter bacteria associated with milk. In several research and quality programs, it is very important to develop a rapid and sensitive method for their quantitative determination in dairy products to monitor bacterial growth and activity. A capillary electrophoresis method for the simultaneous determination of oxalic, citric, formic, succinic, orotic, uric, pyruvic, acetic, propionic, lactic, and butyric acid in less than 18 min has been developed. Various parameters affecting analysis, including capillary length, type, composition, and pH of the electrolyte have been optimized. Some alternatives are given to improve the separation of particular organic acids of special interest. Its application to analyze the quality of some dairy products has been investigated. In addition, the suitability of the technique to determine profiles of organic acids generated during the metabolism of heat-shocked spores has been demonstrated.  相似文献   

18.
A rapid method for the determination of 16 elements in tobacco by wavelength dispersive X-ray fluorescence spectrometry has been developed. The method is accurate and precise, and requires only 9 min per sample for quantitation. Sample preparation consists of placing a portion of dried, ground tobacco in a sample cup, and pressing at 25 tons pressure to make a compressed pellet. This pellet is then automatically analyzed by X-ray fluorescence for 16 elements. The results are stored on a computer disk for future recall and report generation.  相似文献   

19.
Evidence is presented that the electrophoretic mobility of the polysaccharide pectin in typical capillary electrophoresis (CE) experiments is determined largely by its chain-averaged charge density, irrespective of how that charge is distributed. This was found to be the case for both high and low calcium sensitive sister fractions separated from a mother sample on the grounds of calcium affinity and for blocky methylester distributions generated by a processive demethylating enzyme. The blockiness of the generated intramolecular methylester distribution was substantiated experimentally, also by CE, by observing the oligomeric digest fragments produced by incubation with endo-polygalacturonase II from Aspergillus niger. The conclusion that the CE migration time is largely invariant to the intramolecular methylester distribution supports the idea that the CE peak shapes can be used to give a useful indication of the intermolecular methylester distribution.  相似文献   

20.
A method has been developed for the determination of beta-propiolactone by derivatizing it to the volatile N-hexyl-3-heptafluorobutanoyloxypropanamide, which can be separated and identified by a capillary CP-Sil 8 column, and detected by an electron capture detector (ECD). First, beta-propiolactone is reacted with N-hexylamine to yield N-hexyl-3-hydroxypropanamide. The fluorobutanoyl ester derivative is next prepared by using heptafluorobutyric acid anhydride in the presence of trimethylamine. The method is very sensitive, simple, and specific, and can be used to detect and quantitate residual beta-propiolactone in lyophilized biological materials. The limit of detection is 0.2 ppm beta-propiolactone in a 50 mg sample; however, because of variability at low levels, the limit of quantitation is 1 ppm. Detector response was linear for 2-500 mg beta-propiolactone. Recoveries were 98% or greater from lyophilized vaccines spiked at the 2-20 ppm level. No side products or interference peaks were observed in the derivatization reaction.  相似文献   

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