Showing papers in "Journal of AOAC International in 1985"

Determination of total dietary fiber in foods and food products: collaborative study.

Abstract: A collaborative study was conducted to determine the total dietary fiber (TDF) content of food and food products, using a combination of enzymatic and gravimetric procedures. The method was basically the same as published earlier (J. Assoc. Off. Anal. Chem. (1984) 67, 1044-1052), with changes in the concentration of alcohol and buffers, time of incubation, sample preparation, and some explanatory notes, all with the intent of decreasing the coefficient of variation (CV) of the method. Duplicate blind samples of soy isolate, white wheat flour, rye bread, potatoes, rice, wheat bran, oats, corn bran, and whole wheat flour were analyzed by 9 collaborators. TDF was calculated as the weight of the residue minus the weight of protein and ash. CV values of the data from all laboratories for 7 of the samples ranged from 1.56 to 9.80%. The rice and soy isolate samples had CV values of 53.71% and 66.25%, respectively; however, each sample contained only about 1% TDF. The enzymatic-gravimetric method for determining TDF has been adopted official first action.

Review of Chromatographic Methods for Chloramphenicol Residues in Milk, Eggs, and Tissues from Food-Producing Animals

Abstract: Although chloramphenicol is not approved for use in food-producing animals in the United States, this broad spectrum antibiotic has been widely used to treat diseases in such animals including the lactating dairy cow. Extremely low ophthalmologic doses of chloramphenicol are known to cause aplastic anemia in humans. The residues in meat, milk, and eggs intended for human consumption cause particular public health concern because the bone marrow aplasia is not dose dependent. Furthermore, chloramphenicol, a known inhibitor of protein synthesis, also retards erythropoiesis, a condition that is dose dependent and may cause allergic hypersensitivity reactions. This paper is a review of sensitive methods that use gas, liquid, thin layer, and simple column chromatography as both determinative and cleanup steps for detecting and quantitating chloramphenicol in edible animal tissues, milk, and eggs.

Pesticides, selected elements, and other chemicals in infant and toddler total diet samples, October 1978-September 1979.

Abstract: The U.S. Food and Drug Administration (FDA) conducts Total Diet Studies to determine the dietary intake of selected pesticides, industrial chemicals, and elements (including radionuclides). These studies involve the retail purchase and analysis of foods representative of the diets of infants, toddlers, and adults. The individual food items are separated into a number of food groups, each of which is analyzed as a composite. This report summarizes the results for infant and toddler Total Diet samples collected in 10 cities between October 1978 and September 1979. The average concentration, range of concentrations, and calculated average daily intake of the chemicals found are presented by food group. The average daily intakes of the chemicals are similar to those found in the several preceding years and generally are within acceptable limits. The results for samples collected during the same period that represent the adult diet are reported separately.

Pesticides, selected elements, and other chemicals in infant and toddler total diet samples, October 1979-September 1980.

Abstract: The U.S. Food and Drug Administration (FDA) conducts Total Diet Studies to determine the dietary intake of selected pesticides, industrial chemicals, and elements (including radionuclides). These studies involve the retail purchase and analysis of foods representative of the diets of infants, toddlers, and adults. The individual food items are separated into a number of food groups, each of which is analyzed as a composite. This report summarizes the results for infant and toddler Total Diet samples collected in 10 cities between October 1979 and September 1980. The average concentration, range of concentrations, and calculated average daily intake of each chemical found are presented by food group. The average daily intakes of the chemicals are similar to those found in the several preceding years and generally are within acceptable limits. The results for samples collected during the same period that represent the adult diet are reported separately.

Antibiotic identification by high voltage electrophoresis bioautography.

Abstract: The high voltage electrophoresis bioautography method is applicable to meat, milk, and animal feeds. Meat is freeze-dried, powdered, and extracted with acetonitrile-water (9 + 1), and the extract is concentrated by evaporation at room temperature. Milk is examined directly or following acetonitrile-water extraction. Feed is extracted with acetonitrile-water. Samples or extracts are applied to preliminary assay plates of antibiotic medium No. 1 at pH 6 and 8, seeded with Micrococcus luteus (ATCC 9341), M. luteus DHSR (ATCC 9341A), Bacillus cereus (ATCC 11778), or B. cereus K250 TR (NCIB 11183), and nutrient agar at pH 7 seeded with B. subtilis BGA. Inactivation of penicillinase indicates beta-lactam antibiotics. Addition of trimethoprim increases sensitivity to sulfonamides. After 18-24 h incubation at 30 degrees C, plates yielding clear inhibition zones guide selection of conditions for subsequent electrophoresis bioautography. Extracts are applied (5-100 microL) to 10 mm diameter wells on electrophoresis plates 60 cm long and 40 cm wide, with a gel depth of 1.6 mm. The support medium is 1% agar and 1% agarose in Tris/succinic acid buffers pH 6 and pH 8. A potential of 1500 V is applied for 1.5 h at 15 degrees C. Following electrophoresis, the migrated antibiotics are visualized by over-layering with antibiotic medium No. 1, pH 6 or 8, seeded with M. luteus or B. cereus spore suspension; plates are incubated for 18-24 h at 30 degrees C. Identification is based on results of preliminary screening together with electrophoretic migration distances and inhibition zone appearances compared with standards.

Multiresidue method for quantitative determination of organophosphorus pesticides in foods.

Abstract: A multiresidue method for the quantitative determination of organophosphorus pesticides in foods from the Food and Drug Administration's Total Diet Study is described. The organophosphorus pesticides are separated on the basis of polarity and determined in both fatty and nonfatty foods with a minimum of interferences. The foods analyzed included raw and cooked individual foods as well as combination dishes, water, and whiskey. Recoveries of 17 organophosphorus pesticides in 41 foods ranged from about 80 to 118%.

Gas chromatographic determination of picloram in fish.

Abstract: A simple method for determining picloram in fish is described. The sample is homogenized with ethyl acetate, acidified with 1N HCl, and extracted twice more with ethyl acetate. Ethyl acetate fractions are pooled, derivatized with diazomethane, cleaned up by column chromatography, and analyzed by electron capture gas chromatography. Rainbow trout exposed to 14C-picloram were used to evaluate the efficiency of 2 methods of extraction and to provide data on the rate of uptake and the bioconcentration factor. The detection limit for this method is 5 ng/g, using a 4 g sample.

Capillary gas chromatographic determination of some chlorobiphenyls in eel fat: interlaboratory study.

Abstract: A method for determination of 6 individual chlorobiphenyls in eel fat, based on saponification of the sample and determination with capillary gas chromatography, was studied collaboratively. Eleven laboratories submitted analytical results in duplicate for 6 individual chlorobiphenyls on 2 naturally contaminated eel fat samples. The reproducibility coefficient of variation was about 14% at the 1 mg/kg level for each chlorobiphenyl compound and about 23% at the 0.1 mg/kg level. For each compound, the mean recovery was about 90% with a standard deviation varying from 7 to 9%.

Atomic absorption spectrophotometric determination of liver copper: collaborative study.

Abstract: Eleven collaborating laboratories conducted replicate analyses on 4 blind duplicate pairs of bovine liver samples that either had naturally acquired copper levels or were spiked with one of 3 copper levels. A National Bureau of Standards Bovine Liver sample (SRM 1577, 193 +/- 10 mg copper/kg) and a 1000 mg copper/L standard were also submitted to the collaborators. The method requires the tissue to be digested with concentrated HNO3 at 60 degrees C, diluted to volume with water, and analyzed by atomic absorption spectrophotometry. The intralaboratory coefficients of variation (CVo) ranged from 5.6 to 19%; the interlaboratory CVx values ranged from 7.1 to 21%. The lower limit of detection was estimated to be 1 mg copper/kg tissue. The method has been adopted official first action.

Purge and trap method for determination of ethylene dibromide in whole grains, milled grain products, intermediate grain-based foods, and animal feeds.

Abstract: An improved method has been developed for the determination of ethylene dibromide (EDB; 1,2-dibromoethane) in whole grains, milled grain products, intermediate grain-based foods, and animal feeds. Samples are mixed with water and sparged with nitrogen for 1 h with stirring in a water bath at 100 degrees C. The EDB collected on the adsorbent Tenax TA is eluted with hexane and determined by gas chromatography (GC) with electron capture detection (ECD) and confirmed with Hall electrolytic conductivity detection (HECD) using a second GC column. The highest levels of EDB were also confirmed by full scan GC/mass spectrometry (GC/MS). A total of 24 whole grains, milled grain products, intermediate grain-based foods, and animal feeds analyzed by using this method contained EDB levels up to 840 ppb (wheat). Recoveries from fortified samples ranged from 90 to 105%. Values from this method were compared with those obtained from the acetone soak method; for all 24 samples, this purge and trap method gave equivalent or superior recoveries and detected levels of EDB. Chromatograms for this purge and trap method were clean, enabling a quantitation level of 0.5 ppb to be achieved.

Rapid thin layer chromatographic determination of aflatoxin M1 in powdered milk.

Abstract: A method has been developed for the detection of aflatoxin M1 in milk. The toxin is extracted with chloroform, the extract is evaporated, and the residue is partitioned between carbon tetrachloride and an aqueous saline-methanol solution. The toxin is once again extracted with chloroform from the methanol solution and analyzed by thin layer chromatography. The limit of detection of M1 in powdered milk is 0.5 microgram/kg; recoveries of added M1 are about 83%. The limit of detection can be improved to 0.3 microgram/kg if the plate is sprayed with an aqueous solution of H2SO4 after development.

Determination of phosphine: comparison of rates of desorption by purge-and-trap method and by sulfuric acid treatment.

Abstract: Two methods were compared for quantitative determination of phosphine present on fumigated food and materials. The rate of desorption of PH3 by using a purge-and-trap method was shown to be much slower when compared with sulfuric acid treatment and was also simpler. Application of the modified sulfuric acid treatment for real samples is described.

Gas Chromatographic Determination of Pentachlorophenol in Gelatin: Collaborative Study

Abstract: Eleven collaborators participated in this study of a gas chromatographic method for the determination of pentachlorophenol (PCP) in gelatin. Following acid hydrolysis of a 2 g sample, PCP is extracted with hexane and partitioned into KOH solution. After reacidification, PCP is again extracted with hexane for determination by electron capture gas chromatography on a 1% SP-1240DA column. Three duplicate practice samples (0.0, 0.5, and 1.5 ppm) and 5 blind duplicate collaborative samples (0.0, 0.02, 0.1, 0.5, and 2.0 ppm) were analyzed by each collaborator. Mean recoveries of PCP in the collaborative samples ranged from 88% at the 0.02 ppm fortification level to 102% at the 0.1 ppm level; the overall mean recovery was 96%. Interlaboratory coefficients of variation ranged from 16.4% for the 0.1 ppm fortification level to 22.9% for the 0.5 ppm level; the overall interlaboratory coefficient of variation was 19.5%. The method has been adopted official first action.