Dry rehydratable film for enumeration of total aerobic bacteria in foods: collaborative study

A rehydratable dry-film plating procedure for aerobic plate counts has been compared to the standard agar plate method (966.23B and C, 15th ed.; 46.014-46.015, 14th ed.) in a collaborative study by 12 laboratories. Each laboratory analyzed the normal microflora of 3 samples in duplicate for 6 products. The aerobic plate counts ranged from 1.0 x 10(3) to 1.0 x 10(8) cfu/g. The products were flour, nuts, frozen raw shrimp, spice, frozen raw ground turkey, and frozen and refrigerated vegetables. Repeatability standard deviations of the 2 methods did not differ significantly for 13 of 18 test samples. For 1 shrimp and 2 turkey samples, the dry-film method had lower repeatability variances (P less than 0.05) and for 1 spice sample the agar method had lower repeatability variances (P less than 0.05). Relative standard deviations of repeatability were between 1.7 and 15.5% for the dry-film method and 1.2 and 16.0% for the agar method. Relative standard deviations of reproducibility ranged from 2.4 to 23.4% for the dry-film method and 2.3 to 18.8% for the agar method. The dry rehydratable film method has been adopted official first action for determination of the aerobic plate count.     

Temperature-independent pectin gel method for aerobic plate count in dairy and nondairy food products: collaborative study

Ten laboratories participated in a collaborative study to compare the pectin-based plate count (PC) Redigel method with the aerobic plate count and standard plate count agar-based standard methods for the estimation of total bacterial counts in 9 different nondairy food and dairy food products. The foods were cream, homogenized milk, raw milk, cheese, raw chicken, raw oysters, frozen broccoli, flour, and spices. Each laboratory analyzed 6 samples (3 sample pairs) of each food group. Counts obtained by the pectin-based plate count and agar-based plate count methods differed significantly (P less than 0.05) only for homogenized milk, where the pectin gel method resulted in higher counts. The actual counts were higher in the pectin gel method in 8 of the 9 food groups. The log means for pectin gel and agar-based media, respectively, for the 9 food groups were: cream 8.106 and 7.844; homogenized milk 8.642 and 8.231; raw milk 8.711 and 8.423; chicken 7.654 and 7.645; oysters 7.201 and 7.180; broccoli 7.102 and 6.798; cheese 8.045 and 8.055; flour 4.112 and 3.988; spice 5.379 and 5.314. The repeatability standard deviations favored the pectin gel method in 6 of the 9 foods tested. The reproducibility standard deviations favored the pectin gel method in 7 of the 9 foods tested. These results strongly support the suitability of the pectin gel method as an alternative to agar-based plate count and other methods for total bacterial counts in nondairy and dairy food products. The pectin gel method has been adopted official first action.     

Temperature-independent pectin gel method for coliform determination in dairy products: collaborative study

Ten laboratories participated in a collaborative study to compare a pectin-based violet red bile (VRB) method with the VRB agar-based standard method for estimation of coliform bacterial counts in 7 different dairy food groups: cream, cheddar cheese, cottage cheese, homogenized milk, raw milk, sour cream, and yogurt. Each laboratory analyzed 8 samples of each food group as sample pairs prepared at high, medium, and low inoculum levels, and an uninoculated control pair. Overall mean log counts were higher for the pectin gel method in 18 of 21 cases (7 samples at 3 inoculum levels); 12 results were significantly higher (P less than 0.01) than those for the VRB agar method. Of the 3 higher VRB agar method means, 2 were not significant at P less than 0.10, and one was of borderline significance (0.05 less than P less than 0.06). Repeatability variation (sr) favored the pectin gel method in 14 of 21 cases; 7 were highly significant differences (P less than 0.01). None of the 7 results favoring the VRB agar method was statistically significant. Reproducibility variation (sR) favored the pectin gel method in 14 of 21 results. These data indicate that the pectin gel method gives higher recovery of coliforms with better precision than does the VRB agar method, and strongly support the suitability of the pectin gel method as an alternative to the agar-based VRB method for coliform counts in dairy products. The pectin gel method has been adopted official first action.     

Comparison of Babcock and ether extraction methods for determination of fat content of milk: collaborative study

Eleven collaborating laboratories analyzed 18 blind duplicate pairs of raw milk samples for fat by the Babcock method and by a modified Mojonnier ether extraction method in 7 round robins conducted over a 14 month period. Ten laboratories used the Babcock method and 10 used the modified Mojonnier method. Fat content of samples ranged from approximately 2.7 to 5.6%. Mean test value of samples analyzed was approximately 3.9% fat. Average standard deviations of within-laboratory repeatability (Sr) of the Babcock and ether extraction methods were 0.029 and 0.015% fat, respectively. Average standard deviations of between-laboratory reproducibility (SR) of the Babcock and ether extraction methods were 0.039 and 0.020% fat, respectively. Average repeatability relative standard deviations (RSDr) for the Babcock and ether extraction methods were 0.742 and 0.396%; average reproducibility relative standard deviations (RSDR) were 1.014 and 0.512%, respectively. Mean repeatability values (r) and reproducibility values (R) were 0.081 and 0.111% for Babcock and 0.044 and 0.056% for ether extraction, respectively. The ether extraction method demonstrated consistently better within- and between-laboratory agreement. The overall mean test value for the Babcock method was significantly higher (0.021% fat) than that for ether extraction. The difference between Babcock and ether extraction fat test results was different for different farms. In addition, the mean difference between percent fat determined by the Babcock and ether extraction methods was different in different months. There was no correlation in the difference between Babcock and ether extraction methods with the absolute level of fat in the samples in the range of 2.7 to 5.6% fat. The modifications of the AOAC Babcock method and the modified Mojonnier ether extraction method have been approved interim official first action.     

Comparison of two methods for determination of total solids content of milk: collaborative study

Ten laboratories analyzed 9 pairs of blind duplicate raw milk samples for total solids. A direct forced air oven method (4 h at 100 degrees C) and a modification of the AOAC predry method (16.032) were used. Preliminary evaluation of the modified AOAC method indicated that blank determinations were necessary. Total solids content ranged from 12.0 to 14.6%. Average repeatability standard deviations (Sr) of the direct forced air oven and modified AOAC methods were 0.019 and 0.017, respectively. Average reproducibility standard deviations (SR) of the direct forced air oven and the modified AOAC methods were 0.042 and 0.047, respectively. Average repeatability relative standard deviations (RSDr) for the direct forced air oven and the modified AOAC methods were 0.149 and 0.136%, respectively; average reproducibility relative standard deviations (RSDR) were 0.327 and 0.370%, respectively. Mean repeatability values (r) and reproducibility values (R) were 0.054 and 0.118 for the direct forced air oven method and 0.049 and 0.133 for the modified AOAC method, respectively. The mean test result of the direct forced air oven method (12.7293%) was comparable to that for the modified AOAC method (12.7273%). The modification of AOAC method 16.032 and the direct forced air oven method have been approved interim official first action.     

Combination of total solids determined by oven drying and fat determined by Mojonnier extraction for measurement of solids-not-fat content of raw milk: collaborative study

Each of 9 laboratories analyzed 9 pairs of blind duplicate raw milk samples for fat, using the Mojonnier ether extraction method (16.E13-16.E17), and for total solids, using a new direct forced air oven method. Solids-not-fat was determined by subtracting percent fat from percent total solids. The solids-not-fat content of the samples tested in the collaborative study ranged from 8.48 to 9.36%. The average repeatability standard deviation (sr) and the average reproducibility standard deviation (SR) for the solids-not-fat method were 0.019 and 0.041, respectively. Average repeatability (RSDr) and reproducibility (RSDR) relative standard deviations were 0.218 and 0.466%, respectively. The mean repeatability value (r) was 0.055; the mean reproducibility value (R) was 0.117. The difference between milk total solids determined by direct forced air oven drying and milk fat determined by Mojonnier ether extraction has been approved for interim official first action for determination of solids-not-fat content of milk.     

Dry rehydratable films for enumeration of coliforms and aerobic bacteria in dairy products: collaborative study

A collaborative study was conducted to compare proposed dry-film plating methods, using aerobic count plates and coliform count plates, to standard agar plating methods for quantifying aerobic bacteria and coliforms in dairy products. In this study, 5 food products (chocolate milk, pasteurized cheese, nonfat dry milk, evaporated milk, and vanilla ice cream), selected as representative dairy products, were analyzed by 11 collaborating laboratories. The results indicate that the dry-film plating methods are equivalent to or better than the agar plating methods. The aerobic count and coliform count dry-film plating methods have been adopted official first action.     

Development of a new methanethiol quantification method using ethanethiol as an internal standard

Development of a new method to quantify methanethiol in which ethanethiol was employed as an internal standard is reported. Recovery yields for methanethiol from an aqueous model system and a soy protein concentrate (SPC) aqueous slurry determined with this method ranged from 97 to 107% and from 103 to 121%, respectively. The methanethiol content of two commercial SPCs and two commercial soy protein isolate (SPI) samples, on a dry basis, ranged from 835 to 1190 times greater than the odor threshold for methanethiol. Relative standard deviations for quantifying methanethiol with the method from these samples were <5%, indicating its good reproducibility in quantifying methanethiol from soy protein products. Also investigated in the current study was the feasibility of using 5',5-dithiobis(2-nitrobenzoic acid) (DTNB, Ellman's reagent) to determine the concentration of methanethiol in the aqueous solutions used to prepare the standard curve for quantifying methanethiol from soy protein products. The concentrations of methanethiol obtained from Ellman's reagent method were comparable with those from a weighing method and theoretical calculation.     

土壤水分、有机质和总氮含量的近红外光谱分析研究

本文首次采用了近红外光谱分析法对我国黄土区土壤水分,有机质和总氮含量进行主人分析。结果表明,该法与实验室化学分析法之间相关性高,误差小,５２份样品定标结果：水分,有机质和总氮的复合相关系数分别为０．９７４,０．９３８和０．９４２;标准误差分别为１．０８,０．２３和０．０４２。７４份样品的检验结果;相关系数分别为０．９６９,０．９２１和０．９２８;估测标准误差分别为１．１４,０．２８和０．０４６。三     

Immunodiffusion screening method for detection of motile Salmonella in foods: collaborative study

A collaborative study was performed to validate the performance of the 1-2 TEST for detection of motile salmonellae in foods. Detection is based on observation of an immobilized band of cells. Twenty-three laboratories participated in the study. The 1-2 TEST (immunodiffusion test) was compared with the standard culture procedure (BAM/AOAC; FDA Bacteriological Analytical Manual) for detection of Salmonella in 6 food types: ground black pepper, soy flour, dried whole egg, milk chocolate, nonfat dry milk, and raw deboned turkey. Uninoculated and inoculated samples were included in each food group analyzed. After the tests on the 6 foods were completed, analysis of the data for turkey and soy flour showed that certain collaborators obtained data inconsistent with the data from the majority of collaborators. No specific method deviations to account for the inconsistencies were reported by those collaborators, so the collaborative testing of these 2 foods was repeated. Analysis of data for pepper, chocolate, nonfat dry milk, dried whole egg, and the second set of soy flour and turkey indicated 96.1% agreement between the BAM/AOAC and immunodiffusion test methods. The false negative rates for the immunodiffusion test and BAM/AOAC methods were 3.6 and 1.7%, respectively. There was no significant difference in the productivity of the immunodiffusion test and BAM/AOAC method at the 5% level for any of the 6 foods. The immunodiffusion screening method has been approved official first action for detection of motile Salmonella in foods.     

Electrothermal atomic absorption spectrometric determination of selenium in foods and diets

The validity of 2 electrothermal atomic absorption spectrometric methods for determination of selenium in foods and diets was tested. By using 0.5% Ni(II) as a matrix modifier to prevent selenium losses during the ashing step, it was shown that selenium can be determined in samples containing greater than or equal to 1 microgram Se/g dry wt without organic extraction. The mean recovery tested, using NBS Bovine Liver, was 98%; recovery of added inorganic selenium in Bovine Liver matrix was 100%. In addition, this method gave values closest to the median value of all participating laboratories using hydride generation AAS or the spectrofluorometric method in a collaborative study on high selenium wheat, flour, and toast samples. For samples with concentrations less than 1 microgram Se/g dry wt, separation of selenium from interfering Fe and P ions by organic extraction was necessary. Using inorganic 75Se in meat and human milk matrixes, an ammonium pyrrolidine dithiocarbamate-methyl isobutyl ketone-extraction system with added Cu(II) as a matrix modifier yielded the best extraction recoveries, 97 and 98%, respectively. Accuracy and precision of the method were tested using several official and unofficial biological standard materials. The mean accuracy was within 4% of the certified or best values of the standard materials and the day-to-day variation was 9%. The Se/Fe or Se/P interference limits proved to be low enough not to affect selenium determinations in practically all foods or diets. The practical detection limit of the method was 3 ng Se/g dry wt for 1.0 g dry wt samples.(ABSTRACT TRUNCATED AT 250 WORDS)     

Analytical method for the determination of cyromazine and melamine residues in soil using LC-UV and GC-MSD

A method is reported for the determination of cyromazine and melamine residues in soil. Soil samples are extracted twice via mechanical shaking, each time with 70% acetonitrile/30% 0.050 M ammomium carbonate for 30 min. An aliquot portion of the pooled extracts is subjected to strong cation exchange (SCX) purification on AG 50W-X4 resin. Final analysis is accomplished using liquid chromatography-ultraviolet (LC-UV) detection at a wavelength of 214 nm. Confirmatory analyses can be performed using gas chromatography-mass selective detection (GC-MSD) in the selected ion monitoring (SIM) mode. The limit of detection (LOD) is 2.5 ng injected and the limit of quantification (LOQ) is 10 ppb when using LC-UV for the analysis of N-cyclopropyl-1,3,5-triazine-2,4, 6-triamine (cyromazine) and 1,3,5-triazine-2,4,6-triamine (melamine). The LOD is 0.050 ng injected and the LOQ is 10 ppb when using GC-MSD for confirmatory analyses. The mean procedural recoveries were 97 and 95% and the standard deviations were 16 and 11% for cyromazine and melamine, respectively (n = 24), when using LC-UV. The mean procedural recoveries were 107 and 92% and the standard deviations were 9.9 and 16% for cyromazine and melamine, respectively (n = 29), when using GC-MSD. The method validation study was conducted under U.S. EPA FIFRA Good Laboratory Practice Guidelines 40 CFR 160. The method also passed an Independent Laboratory Validation (ILV) as per U.S. EPA FIFRA Subdivision N.     

Chloramphenicol extraction from honey, milk, and eggs using polymer monolith microextraction followed by liquid chromatography-mass spectrometry determination

A rapid confirmatory method for monitoring chloramphenicol (CAP) residues in honey, whole milk, and eggs is presented. This method is based on the polymer monolith microextraction (PMME) technique and high-performance liquid chromatography (HPLC)-electrospray ionization mass spectrometry (MS). A poly(methacrylic acid-ethylene glycol dimethacrylate) monolithic capillary column was selected as the extraction medium. To obtain optimum extraction efficiency, several parameters related to PMME were investigated. After dissolution in 20 mM phosphate solution at pH 4.0 and centrifugation, honey, eggs, or milk samples were directly passed through the extraction tube. The LC-MS instrument was equipped with an electrospray ion source and a single quadrupole. The eluates were analyzed by LC-MS in the negative-ion mode and by monitoring a pair of isotopic ions for the target compound. The in-source collision-induced dissociation process produced confirmatory ions. The recoveries of CAP from real samples spiked at 0.1-10 ng/g (honey), 0.2-10 ng/mL (milk), and 0.2-10 ng/g (egg) were in the range of 85-102%, with relative standard deviations ranging between 2.1% and 8.9%. The limits of detection (S/N = 3) were 0.02 ng/g, 0.04 ng/mL, and 0.04 ng/g in honey, milk, and eggs, respectively. The proposed method was proved to be robust in monitoring CAP residue in honey, milk, and eggs.     

Comparison of spectroscopic techniques for the determination of Kjeldahl and ammoniacal nitrogen content of farmyard manure

The feasibility of determining the nitrogen content of farmyard manure using infrared spectroscopy was investigated. Fifteen samples each of cattle, pig, and turkey manure were analyzed by three infrared techniques: Fourier transform mid-infrared (MIR), using attenuated total reflection (ATR); near-infrared reflectance (NIR-R); and near-infrared optothermal photoacoustic (NIR-OT). The near-infrared measurements were made at wavelengths determined respectively by four (NIR-OT) and five (NIR-R) band-pass filters. The total nitrogen (using the Kjeldahl method) and volatile (ammoniacal) nitrogen contents of all samples were measured by wet chemistry. Internally cross-validated (ICV) partial least-squares (PLS) regression was then used to obtain calibrations for the nitrogen content. The data sets obtained by each technique were treated separately. Within these sets, data from each manure type were treated both separately and combined: the best predictive ability was obtained by combining data from all three manure types. From the combined data set, the residual standard deviations and correlation coefficients for the ICV-predicted versus actual Kjeldahl nitrogen content were, respectively, 6772 mg/kg dry wt, 0.862 (MIR); 9434 mg/kg dry wt, 0.771 (NIR-OT); and 8943 mg/kg dry wt, 0.865 (NIR-R). For the ammoniacal nitrogen content, the residual standard deviations and correlation coefficients were 3869 mg/kg dry wt, 0.899 (MIR); 6079 mg/kg dry wt, 0.820 (NIR-OT); and 3498 mg/kg dry wt, 0.961 (NIR-R).     

A simple and sensitive liquid chromatography-mass spectrometry confirmatory method for analyzing sulfonamide antibacterials in milk and egg

A simple and specific method able to identify and quantify traces of 14 sulfonamide antibacterials (SAs) in milk and eggs is presented. This method uses a single solid-phase extraction (SPE) cartridge for simultaneous extraction and purification of SAs in the above matrices. Milk and egg samples are passed through a Carbograph 4 sorption cartridge. After analyte desorption, an aliquot of the final extract is injected into a liquid chromatography-mass spectrometry (LC-MS) instrument equipped with an electrospray ion source (ESI) and a single quadrupole. MS data acquisition is performed in the positive-ion mode and by a time-scheduled multiple-ion selected ion monitoring program. Compared to two published methods, the present protocol extracted larger amounts of SAs from both milk and egg and decreased the analysis time by a factor of 3 with milk samples and by a factor of 2 with egg samples. Recovery of SAs in milk at the 5 ppb level ranged between 76 and 112% with relative standard deviations (RSDs) of 相似文献   

Enzymatic-ultraviolet method for measuring lactose in milk: collaborative study

Collaborators in 8 dairy and food industry laboratories performed one lactose determination on each of 8 unknown samples of milk, lowfat milk, or skim milk, as 3 pairs of blind duplicates. Two known samples were provided to gain experience prior to analysis of the unknown samples. All of the above samples were also analyzed for lactose content by the official AOAC gravimetric method (16.507) by a commercial laboratory. From the overall mean of results on all samples, determinations by the enzymatic method averaged 0.49% lower than by the AOAC method. This difference was significant by the t-test (P = 0.05), which indicated a lack of agreement between the compared methods in determining lactose content. Standard deviations were similar for the 3 sets of blind duplicates which ranged between 3.67 and 4.55% lactose content. F-values revealed that variations between means obtained by laboratories differed significantly as compared with variations within laboratory means. The method has been adopted official first action.     

DNA hybridization assay for detection of Salmonella in foods: collaborative study

A collaborative study was performed in 11 laboratories to validate a DNA hybridization (DNAH) procedure for detection of Salmonella in foods. The DNAH procedure was compared to the standard culture method for detection of Salmonella in 6 foods: ground pepper, soy flour, dry whole egg, milk chocolate, nonfat dry milk, and raw deboned turkey. With the exception of turkey which was naturally contaminated, uninoculated and inoculated samples of each food group were analyzed. Results for the DNAH method were significantly better than for the standard culture method at the 5% probability level for the detection of Salmonella in turkey. There was no significant difference between the methods for the other 5 foods. The method has been adopted official first action.     

Quantitation of added water in milk by using vapor pressure osmometry

A vapor pressure osmometer (VPO) was successfully studied in 1975. An improved osmometer with greater range and temperature stability was evaluated. Repeatability on 290 mOs/kg standard solution was 289.5 +/- 1.08. The mean and standard deviation on 36 water-free milk samples was 280.5 +/- 4 compared to 280.1 +/- 3 in the previous study. Instrument data from 2 osmometers and 2 cryoscopes produced acceptable chi-square values, and the correlation coefficients between methods were better than 0.99 for samples containing 1--21% added water. In a survey involving 760 samples, more than 37% of producer samples in one cheese plant contained greater than 3% added water. Additional evidence of added water in market milk samples suggests the immediate application of the VPO to help prevent milk adulteration. The vapor pressure osomometer method for quantitating added water in milk has been adopted as official first action.     

In vivo rat assay for true protein digestibility: collaborative study

Eight laboratories participated in a collaborative study to estimate precision of a standardized rat assay for determining true protein digestibility in selected animal, fish, and cereal products. Each of 7 test protein sources (casein, tuna fish, macaroni/cheese, pea protein concentrate, rolled oats, pinto beans, and nonfat dried milk) was fed as the sole source of protein at a 10% protein level in mixed diets. Each diet was fed to 2 replicate groups of 4 rats each for a 4-day acclimation period and a 5-day balance period. Mean digestibilities ranged from 98.6% for casein to 72.6% for pinto beans. Repeatability standard deviations ranged from 0.5 to 2.0%; the mean relative standard deviation for repeatability was 0.9% (range 0.5-2.8%). Reproducibility standard deviations ranged from 1.2 to 3.2%, and the mean relative standard deviation for reproducibility was 2.4% (range 1.3-4.4%). The method has been approved interim official first action for determining true protein digestibility in foods and ingredients.     

Gamma-ray spectroscopic determination of iodine-131 and cesium-137 in foods: two collaborative studies

The AOAC method for iodine-131, cesium-137, and barium-140 in milk by gamma-ray spectroscopy (48.025-48.029) was extended to include other foods for the radionuclides iodine-131 and cesium-137. Two collaborative studies were performed to validate this extension. In the first study, a food sample containing 119 pCi 131I/kg and 53 pCi 137Cs/kg was sent to each of 45 laboratories for triplicate analyses. For 25 responses, the mean of the reported values was 123.8 pCi/kg for iodine-131, and for 27 responses, the mean was 53.4 pCi/kg for cesium-137. Repeatability (within-laboratory) standard deviations (Sr) for iodine-131 and cesium-137 were 4.6 and 3.7 pCi/kg, respectively. Reproducibility (among-laboratories) standard deviations (SR) for iodine-131 and cesium-137 were 12.1 and 6.0 pCi/kg, respectively. In the second study, a food sample containing 25 pCi 131I/kg and 27 pCi 137Cs/kg was sent to each of 54 laboratories for triplicate analyses. For 21 responses, the mean of the reported values was 25.0 pCi/kg for iodine-131, and for 19 responses, the mean was 28.9 pCi/kg for cesium-137. Sr Values were 4.0 and 1.6 pCi/kg for iodine-131 and cesium-137, respectively, and SR values were 5.0 and 2.8 pCi/kg, respectively. The method extension was adopted official first action.