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1.
A tri-enzyme digestion procedure using chicken pancreas conjugase, alpha-amylase, and Pronase was evaluated to determine its usefulness in the microbiological quantitation of total folate in foods. Folate values obtained by traditional conjugase digestion were compared to those obtained by the tri-enzyme method for 12 food products that represent diverse matrixes. The tri-enzyme treatment increased measurable folate from most foods when compared to levels found after conjugase digestion. Largest increases were noted for tuna fish (51%) and yogurt (33%) after tri-enzyme digestion. For the 12 foods, a mean increase of 19% in measurable folate was obtained with tri-enzyme treatment. The study shows that traditional conjugase treatment does not completely free folate from complex food matrixes before microbiological analysis. Further, as other investigations have suggested, current accepted methods for folate analysis may be underestimating folate levels in foods.  相似文献   

2.
A trienzyme treatment (protease, alpha-amylase, and human plasma conjugase), followed by purification using SPE with SAX cartridges and reversed-phase HPLC with UV-PDA detection, was performed for determination of the distribution of various folate forms and content at various stages of tempe preparation. The major folate form in soybean identified was 5-formyl tetrahydrofolate (5-CHO-H4folate), followed by 10-formyl tetrahydrofolate (10-CHO-PGA), and 5-methyl tetrahydrofolate (5-CH3-H4folate), whereas folic acid was not detected and tetrahydrofolic acid (H4folate) was not detectable. The most predominant form in tempe was also 5-CHO-H4folate, followed by 10-CHO-PGA, whereas the quantities of 5-CH3-H4folate and folic acid were negligible. Quantities and retention of folate significantly decreased during the first boiling, dehulling, soaking, and second boiling procedures, yielding folate retention of 32%. A remarkable increase in folate content was found after fermentation, 5.2-fold higher than that of the boiled soybean. This may be due to de novo formation of folate by Rhizopus oligosporus, the principal mold in tempe fermentation. HPLC results were approximately 38-55% lower than the values obtained from the microbiological assay using Lactobacillus casei.  相似文献   

3.
In 1989, the Community Bureau of Reference started a research program to improve the quality of vitamin analysis in food. To achieve this task, vitamin methodology was evaluated and tested by interlaboratory studies and the preparation of certified reference materials, which will be used for quality control of vitamin measurements. The main improvements in methodology were achieved by testing and standardizing the extraction condition and enzymatic hydrolysis procedures. Results for each individual material are derived from five replicate determinations using at least two independent methods: liquid chromatography (HPLC) and microbiological assay for vitamins B1, B2, and B6; and radioprotein binding and microbiological assays for vitamin B12. The certificate of analysis for four reference materials gives mass fraction values for water-soluble vitamins. These certified values were based on the acceptable statistical agreement of results from collaborating laboratories. Certified values with uncertainties (mg/kg dry matter) for each CRM are as follows: 4.63 (0.20) and 4.10 (0.51) for vitamins B1 and B6, respectively, in CRM 121 (wholemeal flour); 6.51 (0.24), 14.54 (0.3), 6.66 (0.43), and 0.034 (0.003) for vitamins B1, B2, B6, and B12, respectively, in CRM 421 (milk powder); 3.07 (0.17) and 4.80 (0.40) for vitamins B1 and B6, respectively, in CRM 485 (lyophilized mixed vegetables), and 8.58 (0.55), 106.8 (2.8), 19.3 1.5), and 1.12 (0.044) for vitamins B1. B2, B6, and B12, respectively, in CRM 487 (lyophilized pig liver).  相似文献   

4.
Twelve popular ready‐to‐eat breakfast cereals fortified with folic acid were sampled in the United States in 2006, and the data have been incorporated into the USDA National Nutrient Database for Standard Reference. Cereals were collected from three statistically selected retail outlets in each of four primary census regions, and four composites of each product were prepared using random groupings of three locations each. Folic acid was determined using a validated LC‐MS method, with 13C‐folic acid as an internal standard, after trienzyme treatment and solid phase extraction. A cereal reference material (AACC VMA399) was analyzed as a control. Selected samples were also assayed using the standard microbiological method, with and without trienzyme extraction, to generate an estimate of endogenous folate. On average, as shown on the label, folate content was underestimated. In seven cereals, folate was within 5% of the declared value; in four cereals, it was 5–20% higher; and in two cereals, it was >20% greater, representing –75 to +69 μg/serving (mean 17) of the label value, equivalent to –19% to +17% of the 400 μg/daily value. The microbiologically determined folic acid was higher than LC‐MS by 10–67% (mean 40%). Therefore, use of label values might underestimate folate intake from some breakfast cereals.  相似文献   

5.
Over the past two decades, the role of folate in human nutrition has been of much interest because of its relationship to diseases such as neural tube defects and heart disease. Since 1998, the U.S. Food and Drug Administration has mandated that cereal products be fortified with 140 microg of folic acid/100 g. It is important, therefore, to be able to determine accurately the folate concentrations in cereals and other grains to ensure proper dietary intake of folate. In this study, a microbiological method employing a trienzyme extraction procedure was applied to the analysis of folate in several starchy grain legumes (pulses). Differences in the folate content of dry bean were observed among some market classes but not between cultivars in the same market class. Location had a significant effect on the folate content of lentil and dry pea; cultivar did not. The significant effect of market class, cultivar, and growth environment on the levels of folate in pulses is of particular importance to pulse processors and pulse breeders.  相似文献   

6.
Two automated fluorometric methods were compared with the official AOAC methods for determining vitamin C in fortified ready-to-eat cereals, fruits, vegetables, baby foods, flour products, pet foods, meats, frozen dinners, juices, and nutritional health bars. Each sample was analyzed in duplicate on 2 days and included a recovery study on all products. Egberg's semiautomated method (Method 1) and Roy's automated method (Method 2) were compared with the manual AOAC tritrimetric and fluorometric methods. The correlation factor for Methods 1 and 2 were 0.999 and 0.979, respectively, when compared with the AOAC methods. The recovery study showed average recoveries of 97.8% for Method 1, 99.3% for Method 2, and 100.6% for the AOAC methods. The results suggest that Method 1 is the method of choice for the majority of the products analyzed.  相似文献   

7.
A simplified HPLC method for rapid determination of folates in yeast with ultraviolet and fluorescence detection without sample purification has been developed. By use of the column Aquasil C(18), specially designed for polar analytes, and gradient elution, it was possible to separate and determine five folate derivatives: tetrahydrofolate, 5-methyltetrahydrofolate, and 5-formyltetrahydrofolate with fluorescence detection, and 10-formylfolic acid and folic acid with ultraviolet detection. The sample preparation required only a small amount of dry yeast (25-50 mg) and included an extraction of folates by heat treatment and deconjugation of folate polyglutamates to monoglutamates with the use of rat serum conjugase. Validation involved investigation of matrix effects, determination of recovery by standard addition method, repeatability, and stability tests. The dominating folate forms in commercial dry baker's yeast were found to be tetrahydrafolate and 5-methyltetrahydrofolate with a total folate content of 2890 microg/100 g (63.4 nmol/g). The simplicity of the method makes it suitable for folate screening studies of different yeast strains.  相似文献   

8.
A gas chromatographic (GC) method for determination of supplemental alpha-tocopheryl acetate in high potency vitamin E powders and oils was collaboratively studied as an alternative to the AOAC colorimetric method (43.147-43.151, Emmerie-Engel), which requires saponification, extraction of the saponifiable fraction, and quantitation by colorimetry. The simpler GC procedure requires only extraction and/or enzymatic digestion and dilution before quantitation. Six blind duplicates were distributed to 10 laboratories; all 10 returned results. Repeatability (sr) and reproducibility (sR), % vitamin E/g, for the feed oil concentrates was 1.1 and 1.3, respectively; for the feed adsorbates 1.0 and 1.5; and for the spray-formulated powders 1.4 and 1.3. These results compare favorably with results obtained in a comparison study of the GC and Emmerie-Engel methods conducted by BASF in 1985. The method has been approved interim official first action for determination of alpha-tocopheryl acetate in vitamin E acetate concentrates as an alternative for those products only to AOAC colorimetric method 43.147-43.151.  相似文献   

9.
The essentiality of dietary folates for human beings has been known for many years. Over the shorter term, biological activities associated with several human maladies and the attenuation of biomarkers for several chronic diseases also have been assigned to folates. In the United States, these observations have led to the addition of folic acid to several foods and food ingredients (food fortification) and to dietary recommendations that assign biological activity to each of the forms of folate in the food supply. There currently is unavailable a robust, instrumental procedure that will distinguish between naturally occurring food folates and synthetic folic acid as part of the routine analysis of foods. The procedure proposed in this publication is unique in that it uses "off-the-shelf" supplies and instrumentation, to the extent possible, and was developed with "normal" corporate work schedules in mind. This method takes advantage of the tri-enzyme food digestion and folate deconjugation steps but was optimized with a commercially available rat plasma as the source of conjugase. A high-capacity styrene-divinylbenzene-based solid-phase extraction column was identified, and conditions were developed for quantitative recovery of 5-methyltetrahydrofolate and folic acid (FA) with it. The various forms of food folates are separated on a C-18 high-performance liquid chromatography (HPLC) column which is resistant to degradation at low pH. As a result, the mobile phase was simplified to a gradient of low-pH phosphate buffer (pH 2.2) and acetonitrile. Although FA does not exhibit fluorescence, a UV-induced photolysis system was added, which is controlled by the HPLC system, so that an appropriate segment of the HPLC column effluent is subjected to photolytic conditions and, thereby, FA can be measured as a fluorescent product. The application of the system was verified by analyzing several certified reference materials and foods and comparing results with certified values and/or total folate values as determined by microbiological assay.  相似文献   

10.
The effect of baking method on folates of rye and wheat breads, as well as the effect of sourdough fermentation of rye, were examined. Sourdough fermentations were performed both with and without added yeast, and samples were taken throughout the baking process. Samples were analyzed microbiologically for their total folate content after trienzyme extraction. Individual folate vitamers were determined by HPLC after affinity chromatographic purification. The lowest folate contents for both rye and wheat breads were found from breads baked without added yeast. Total folate content increased considerably during sourdough fermentation due to increased amounts of 10‐HCO‐H2folate, 5‐CH3‐H4folate, and 5‐HCO‐H4folate. Baker's yeast contributed markedly to the final folate content of bread by synthesizing folates during fermentation. Proofing did not influence total folate content but changes in vitamer distribution were observed. Folate losses in baking were ≈25%. The variety of sourdoughs and baking processes obviously lead to great variation in folate content of rye breads. The possibilities to enhance natural folate content of rye bread by improving folate retention in technological processes and by screening and combining suitable yeasts and lactic acid bacteria should be further investigated.  相似文献   

11.
Bioavailability of dietary folate might be impaired by the polyglutamate chain to which approximately 70% of dietary folates are bound. This chain must be removed enzymatically in the intestine before folate is absorbed as a monoglutamate. To increase formation of monoglutamate folate in vegetables, the vegetables were subjected to various processing treatments. Treatments included freezing (-18 degrees C, 16 h) and thawing (4 degrees C, 24 h) and hydrostatic high-pressure treatment (200 MPa, 5 min). Both freezing/thawing and high-pressure treatment increased the proportion of folate in the monoglutamate form in leeks, cauliflower, and green beans 2-3-fold. However, loss of total folate after these treatments was >55%. It is concluded that conversion of folate polyglutamate to the monoglutamate form in vegetables is possible by certain processing treatments. Potentially this could lead to vegetables with higher folate bioavailability. However, to prevent folate loss into processing water, processing in a closed system should be applied.  相似文献   

12.
A comparative study was conducted to evaluate four previously reported methods that proved to have a recovery greater than 80% for the determination of different levels of ochratoxin A (OTA) in green and roasted coffee beans and to select an accurate, sensitive, and less-expensive technique between the existing methods. The results indicated that the Association of Official Analytical Chemists (AOAC) official method for the extraction of OTA in green coffee and determination by high-performance liquid chromatography (HPLC) is recommended as an efficient method for the routine analyses of OTA in green and ground roasted coffee beans. This method proved to be an accurate, sensitive, and less-expensive method that employs routine materials and available equipment. Although the immunoaffinity column/HPLC procedure tested showed a significantly higher percentage than the AOAC recommended method, it is recommended for use in processed coffee beans where low concentrations of OTA may be expected to be detected.  相似文献   

13.
The use of near-infrared (NIR) reflectance spectroscopy for the rapid and accurate measurement of soluble and insoluble dietary fiber was explored in a diverse group of cereal products. Ground samples were analyzed for soluble and insoluble dietary fiber (AOAC Method 991.43) and scanned (NIRSystems 6500 monochromator) to obtain NIR spectra. Modified PLS models were developed to predict insoluble and soluble dietary fiber using data sets expanded to include products with high fat and high sugar contents. The models predicted insoluble dietary fiber accurately with an SECV of 1.54% and an R(2) of 0.98 (AOAC determined range of 0-48.77%) and soluble dietary fiber less accurately with an SECV of 1.15% and an R(2) of 0.82 (AOAC determined range of 0-13.84%). Prediction of independent validation samples by the soluble fiber model resulted in a bias that may be related to the way the reference method treats samples with different soluble fiber constituents. The insoluble fiber model can be used to rapidly monitor insoluble dietary fiber in cereal products for nutrition labeling.  相似文献   

14.
A reversed phase ion-pair liquid chromatographic method for the determination of nicotine in commercial tobacco products was previously developed and optimized (Ciolino, L. A.; Turner, J. A.; McCauley, H. A.; Smallwood, A. W.; Yi, T. Y. J. Chromatogr. 1999a, 852 (2), 451-463) and provided reliable results for the determination of nicotine in commercial moist snuff (Ciolino, L. A.; McCauley, H. A.; Fraser, D. B.; Barnett, D. Y.; Yi, T. Y.; Turner, J. A. J. Agric. Food Chem. 1999b, 47, 3706-3712). The method uses an aqueous-based sample extraction and provides rapid separation of nicotine from the minor tobacco alkaloids and other commercial tobacco components. In the present work, the method is evaluated for the determination of nicotine in commercial cigarettes and compared to both an official AOAC method for total alkaloids in tobacco (AOAC, AOAC Official Methods of Analysis of AOAC International, 16th ed.; AOAC International: Gaithersburg, MD, 1995; pp 30-31), and a published GC method (Lyerly, L. A.; Greene, G. H. Beitr. Tabakforsch. 1976, 8 (6), 359-361). Good agreement was obtained between the ion-pair LC method and the GC method with relative differences in determined nicotine contents of 0.6 to 5% for a series of commercial and reference cigarettes.  相似文献   

15.
The amount of aflatoxin extracted from raw peanuts by using the water-slurry modification of AOAC Method II was determined for 49 different combinations of methanol concentrations and solvent/peanut ratio. Results indicate that the amount of aflatoxins B1 and B2 extracted from raw peanuts is a function of both methanol concentration and solvent/peanut ratio, and a cubic equation was developed, using regression techniques, to describe the combined effects. From the functional relationship, the predicted methanol concentration and solvent/peanut ratio that extracts the most aflatoxin B1 was computed to be 60.0% and 10.8 mL solvent/g peanuts, respectively. This combination extracted 12.1% more aflatoxin than did AOAC Method II.  相似文献   

16.
AOAC method 996.01, used in cereal foods to determine total fat as defined by the U.S. Nutrition Labeling and Education Act (NLEA), is laborious and time-consuming and utilizes hazardous chemicals. Near-infrared (NIR) reflectance spectroscopy, a rapid and environmentally benign technique, was investigated as a potential method for the prediction of total fat using AOAC method 996.01 as the reference method. Near-infrared reflectance spectra (1104-2494 nm) of ground cereal products (n = 72) were obtained using a dispersive spectrometer, and total fat was determined according to AOAC method 996.01. Using multivariate analysis, a modified partial least-squares model was developed for total fat prediction. The model had a SECV of 1.12% (range = 0.5-43.2%) and a multiple coefficient of determination of 0.99. The model was tested with independent validation samples (n = 36); all samples were predicted within NLEA accuracy guidelines. The results indicate that NIR reflectance spectroscopy is an accurate means of determining the total fat content of diverse cereal products for nutrition labeling.  相似文献   

17.
Enzyme-assisted extraction of moniliformin from extruded corn grits   总被引：1，自引：0，他引：1  
Water has been known to be the ideal solvent for moniliformin but is not suitable to extract this toxin from cooked matrices due to instant swelling upon addition of the solvent. In this study, an improved method to extract moniliformin from extruded corn grits using alpha-amylase was developed. In an effort to optimize the method, the efficacy of using a protease was also studied. Treatment with alpha-amylase resulted in a clear solution with decreased suspended solid content as measured by transmittance (%T), which improved from 0 to 96% in 10 min. The detected level of moniliformin from extruded corn grits was increased to 4.02 mug/g when extracted with 1% tetrabutylammonium hydrogen sulfate following alpha-amylase treatment compared to 2.56 microg/g when it was extracted with 90% acetonitrile without enzyme treatment. The average recovery of moniliformin from extruded corn grits was 96% when alpha-amylase was used in the extraction procedure. Overall, the amounts of moniliformin detected in extruded corn grits increased significantly by using enzyme hydrolysis. Chromatographic separation was also benefited by lesser interference and improved peaks.  相似文献   

18.
Gas chromatographic determination of cholesterol in egg products   总被引：2，自引：0，他引：2  
A method has been developed for quantification of cholesterol in fresh egg yolks, spray-dried egg yolks, fresh whole eggs, and spray-dried whole eggs. The method uses saponification followed by petroleum ether extraction of cholesterol. Separation of organic and aqueous layers is enhanced by sodium chloride. Petroleum ether extracts are dried under nitrogen and redissolved in chloroform-methanol (2 + 1) for injection into a gas chromatograph. Cholesterol is separated and quantitated on a high temperature capillary column coated with 5% diphenyl and 95% dimethyl polysilicone crosslinked gum. The method was compared with the current AOAC method 17.017-17.022, and results indicated no significant difference (alpha = 0.05). However, the proposed method allowed separation and analysis of 16 samples in 7 h while the current AOAC method allowed separation and analysis of only 4 samples in 9 h.  相似文献   

19.
Environmental concerns, the disposal cost of hazardous waste, and the time required for extraction in current methods encouraged us to develop an alternate method for analysis of wheat flour lipids. Supercritical fluid extraction (SFE) with carbon dioxide has provided that medium and the method is fully automatic. Crude fats or nonstarch free lipids (FL) were extracted from 4–5 g of wheat flour by an SFE system. To develop optimum conditions for SFE, various extraction pressures, temperatures, and modifier volumes were tried to provide a method that would produce an amount of lipids comparable to those extracted by the AACC Approved Soxhlet Method and the AOCS Official Butt Method using petroleum ether as solvent. Using several wheat flour samples, the best conditions were 12.0 vol% ethanol (10.8 mol%) at 7,500 psi and 80°C to extract the amount of FL similar to those by the AACC and AOCS methods. Using solid‐phase extraction, lipids were separated into nonpolar lipid (NL), glycolipid (GL), and phospholipid (PL) fractions. The mean value of five flours was 1.15% (flour weight, db) by the SFE method, 1.07% by the Butt method, and 1.01% by the Soxhlet methhod. The SFE‐extracted lipids contained less NL and more GL than either the Butt or Soxhlet methods. All three methods extracted lipids with qualitatively similar components. The overall benefit for SFE over the Soxhlet or Butt methods was to increase the number of samples analyzed in a given time, reduce the cost of analysis, and reduce exposure to toxic chemicals.  相似文献   

20.
Abstract

Seven different sample preparation methods (five ashing and fusion methods, an acid digestion method, an oxygen flask combustion method) and the AOAC extraction method (975.04) were compared with a newly developed sealed chamber digestion method for the determination of fluoride (F) in vegetation. Subterranean clover tissue was the test material. Fluoride concentration in digests was measured using a F ion‐selective electrode. The sealed chamber digestion carried out with nitric acid in Teflon chambers at 120°C for 6 hours gave the highest F concentration in the plant material and the highest recovery of added F of all methods. Tests on several types of plant material confirmed the superiority of the closed chamber digestion. The superiority of the method is attributed to the complete solubilisation of F in the sample and elimination of losses of volatile F.  相似文献   

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