Collaborative study of a rapid method for determing aflatoxins in cottonseed products.

Eleven laboratories collaboratively studied a modification of the official final action AOAC method, 26.048-26.056, for determining aflatoxins in cottonseed products. An aflatoxin-negative meal, 6 contaminated meals, 4 contaminated meats (kernels) samples, and 2 ammonia-inactivated meals were used. Mean aflatoxin values, mug/kg, ranged from 6 to 223 (B1), 2 to 44 (B2), and 7 to 266 (total: B1 + B2). Only one laboratory reported a false-positive for the negative meal. The mean coefficients of variation for B1, B2, and total were 28, 56, and 29%, respectively, for meals; 35, 54, and 37%, respectively, for meats; and 35, 58 and 38%, respectively, for ammoniated meals. Statistical treatment of data from triplicate sets of meals and meats showed evidence for systematic error between laboratories. Since the modified method is considerably faster than the official method and yields precision estimates consistent with previous AOAC collaborative studies on determining aflatoxins, the method has been adopted as official first action.     

有机酸和磷对两种污染土壤铅的释放作用研究

用土壤培养和化学浸提法研究了不同低分子量有机酸和磷对污染土壤中铅释放的影响。结果表明,随有机酸浓度增加,铅污染红壤、棕壤中可溶出铅量均增加。当供试有机酸浓度≥1mmol·L-1时,相同浓度有机酸溶出铅量为柠檬酸〉乙酸〉草酸;当有机酸浓度≤0.5mmol·L-1时,溶出铅量为草酸〉柠檬酸〉乙酸。将2g·kg-1磷及50mmol·kg-1有机酸与铅污染红壤以不同方式混合后,柠檬酸处理的溶出铅比率（在污染土壤中加入P、有机酸后溶出铅含量与单加有机酸溶出铅含量之比）为66%（先加有机酸再加磷）、58%（有机酸与磷同时加入）、70%（先加磷再加有机酸）,草酸处理（方式同上）的溶出铅比率为90%、89%、94%,乙酸处理（方式同上）的为10%、8%、10%。铅污染棕壤上,以上处理的溶出铅比率分别为106.46%、104.43%、105.19%（柠檬酸）;43%、48%、58%（草酸）;38%、42%、55%（乙酸）。供试条件下,红壤最低溶出铅比率低于棕壤。     

UV spectrophotometric determination of piperine in pepper preparations: collaborative study

Eight collaborating laboratories performed replicate analyses for piperine on 5 samples representing pepper raw spice, oleoresins, and soluble seasonings. Piperine is extracted into ethylene dichloride and measured at maximal absorbance 342-345 nm with a UV light source. Piperine content is calculated using an absorbance factor derived from piperine. Intralaboratory coefficients of variation (CVo) ranged from 0.5 to 3.1%; interlaboratory coefficients of variation (CVx) ranged from 3.0 to 5.8%. The method has been adopted as an official method of the American Spice Trade Association and as an official first action method by AOAC.     

Environmental Exposure to Cadmium and Lead in the Pediatric Age Group

Lead additives in automotive fuel, smog from a nearby industrial center warranted an investigation on cadmium and lead in Manisa, a city of tabacco processing. Hundred and one children were screened in view of lead and cadmium exposure. In 23 children between the ages of 0–2 years the mean (±SEM) serum lead level was 7.15 ± 0.10 μg/dl, in 28 between the ages of 3–6 years was 7.20 ± 0.10 μg/dl and in 50 between the ages of 7–15 years was 7.20 ± 0.10 μg/dl, respectively, with no significant differences. Serum cadmium levels in the same groups of children was 0.066 ± 0.008 ng/ml, 0.078 ± 0.008 ng/ml 0.088 ± 0.006 ng/ml, respectively. The difference in cadmium levels between the age groups of 0–2 years and 7–15 years was significant (p<0.038). This significant increase in blood cadmium level is also shown by simple linear regression analysis: Cadmium (ng/ml) = 0.049 + 0.005 (age), and p<0.0001, F Ratio = 50.578, coefficient of correlation = 0.581. Our study revealed that lead is not a serious environmental contaminant for children, yet; however, the increasing trend seen in exposure to cadmium warrants serious consideration and urgant preventive measures.     

Influence of automatic dishwashings and scrubbings on release of lead from glazed ceramicware

Use of lead glazes on ceramicware and the release of lead from finished glazes are reviewed. Single units of ceramicware with initial lead leach levels from less than 0.1 to 470 micrograms/mL were subjected to multiple automatic dishwashings with intermediate scrubbing of the ware by plastic fiber pads. Ware was periodically leached with 4% acetic acid solution at room temperature for 24 h, and the solutions were analyzed for lead. Release of lead under these conditions is discussed. Results indicated that neither passive leachings nor multiple dishwashings and scrubbings can predict future lead-release characteristics of glazes and decorations.     

Interlaboratory comparison of analyses for heavy metals in clam tissue

Results are reported for an interlaboratory study conducted to assess the reproducibility of analyses for lead, copper, cadmium, and zinc. The 10 participating laboratories analyzed 2 samples of freeze-dried clam tissue and 1 disguised sample of NBS Oyster Tissue. Interlaboratory variations were observed for all metals, although the methods yielded reproducible data for Cu and Zn with average interlaboratory coefficients of variation of 15 and 11%, respectively. The performance of methods used for Cd and, more so, for Pb was less than satisfactory. Cadmium levels in the 3 samples ranged from about 0.7 to 3.7 ppm with an average interlaboratory coefficient of variation (CV) of 24%. Lead levels in the 3 samples were about 0.5 ppm with an interlaboratory CV of 68%. Some laboratories' results were consistently high or low but data were insufficient to relate these trends to one particular variable. Results from this study were compared with 5 other studies reported in the literature since 1980. Coefficients of variation from all studies were comparable for samples with similar metal concentrations.     

Determination of diagnostic levels of arsenic in animal tissue: collaborative study

The method chosen for this collaborative study is a modification of the AOAC method for As residues, 41.009-41.012. The tissue is dry-ashed overnight at 500 degrees C, and then dissolved in dilute HCl. The solution is diluted and an aliquot is reacted with zinc metal to evolve arsine gas. The gas is trapped in AgDDC solution and As is quantitated at 540 nm. Nine collaborating laboratories performed single analyses on 4 blind duplicate pairs of bovine liver samples which were spiked at 0, 4.3, 10.8, or 21.6 mg As/kg liver. A National Bureau of Standards control (SRM 1566 Oyster Tissue, 13.4 +/- 1.9 mg As/kg) and a 1000 mg As/L standard were also submitted to the collaborators. Intralaboratory coefficients of variation ranged from 7.7 to 17.8%; interlaboratory coefficients of variation ranged from 10.9 to 19.0%. The method has been adopted official first action.     

High pressure liquid chromatographic determination of sodium saccharin, sodium benzoate, and caffeine in soda beverages: collaborative study

A collaborative study for the determination of sodium saccharin, sodium benzoate, and caffeine in 3 types of soda beverage, cola, grape, and lemon-lime, has been completed using reverse phase high pressure liquid chromatography with a muC18 column and acetic acid mobile phase. Recoveries for sodium saccharin were 98.6, 98.0, and 99.1%; for sodium benzoate, 100.6, 102.6, and 100.6%; and for caffeine, 100.8, 101.4, and 101.1%, respectively. The method has been adopted as official first action.     

Determination of zearalenone in corn: collaborative study.

Corn samples spiked at levels of 100, 300, 1000, and 2000 mug zearalenone/kg were sent to 22 collaborators for analysis by the Eppley method. All samples were yellow corn except one white corn sample spiked at 2000 mug/kg. Results from 16 collaborators were statistically analyzed. Only 4 of 16 collaborators detected zearalenone in the sample containing 100 mu/kg, but 11 detected the toxin in the sample containing 300 mug/kg. Average recoveries from all samples were 129% at 300 mug/kg, 101% at 1000 mug/kg, and 88% at 2000 mug/kg. The between-laboratory coefficients of variation were 53.0% at 300 mug/kg, 38.2% at 1000 mug/kg, and 27.0% at 2000 mug/kg. Five naturally contaminated corn samples, one in triplicate, were also provided. The mean level of zearalenone in the naturally contaminated samples ranged from 431 to 7622 mug/kg. The mean coefficient of variation for all samples was 40.5%. Two collaborators measured quantities of zearalenone on thin layer chromatographic plates densitometrically. Their results were not included in the statistical analysis, but the results indicated that densitometric measurement, given proper dilutions of solutions, could be used. The method has been adopted as official first action.     

Comparison of volatile acid number test with enzymatic acetic acid assay for assessment of seafood quality

Volatile acid number, an official AOAC method for assessing seafood quality, was compared with an enzymatic method for measuring acetic acid. Thirty-eight samples of fresh fish and 23 samples of canned fish were evaluated. The data showed high positive correlations between volatile acid number and enzymatic acetic acid methods; the correlation coefficient was 0.98 for fresh fish and 0.95 for canned fish. Positive correlation coefficients of 0.93 and 0.96 were also associated with samples of fish divided into 2 groups on the basis of acceptable or unacceptable quality, respectively. There was no significant difference between the means for the volatile acid number and enzymatic acetic acid procedures at the 5% level of significance. Decomposition studies on cod and mackerel, representing a lean and fatty fish, respectively, were monitored over 9 days by using the following analyses: volatile acid number, acetic acid, total volatile bases, and thiobarbituric acid. Results of the decomposition studies showed that enzymatic acetic acid levels closely paralleled volatile acid number values in both lean and fatty fish. Total volatile bases was a reliable supplemental measure for evaluating lean seafood quality, whereas thiobarbituric acid was more appropriate for further assessment of fatty fish quality.     

Determination of internal insect infestation of oats: collaborative study

An improved method has been developed for determining internal insect infestation of oat kennels. The method involves alcohol defatting and acid hydrolysis of the cracked oats, wet sieving to remove the acid, transfer to a 2 L Wildman trap flask, deaeration by boiling, and treatment with Tween 80-Na4EDTA. Insects are extracted with light mineral oil. Reports from 6 collaborators showed that recoveries averaged 88.98% for adult insect heads and 97.22% for larvae. The method has been adopted official first action.     

Increase in the permeability of tonoplast of garlic (Allium sativum) by monocarboxylic acids

Immersion of intact aged garlic (Allium sativum) cloves in a series of 5% weak organic monocarboxylate solutions (pH 2.0) resulted in green color formation. No color was formed upon treatment with other weak organic acids, such as citric and malic acids, and the inorganic hydrochloric acid under the same conditions. To understand the significance of monocarboxylic acids and their differing function from that of other acids, acetic acid was compared with organic acids citric and malic and the inorganic hydrochloric acid. The effects of these acids on the permeability of plasma and intracellular membrane of garlic cells were measured by conductivity, light microscopy, and transmission electron microscopy. Except for hydrochloric acid, treatment of garlic with all three organic acids greatly increased the relative conductivity of their respective pickling solutions, indicating that all tested organic acids increased the permeability of plasma membrane. Moreover, a pickling solution containing acetic acid exhibited 1.5-fold higher relative conductivity (approximately 90%) as compared to those (approximately 60%) of both citric and malic acids, implying that exposure of garlic cloves to acetic acid not only changed the permeability of the plasma membrane but also increased the permeability of intracellular membrane. Exposure of garlic to acetic acid led to the production of precipitate along the tonoplast, but no precipitate was formed by citric and malic acids. This indicates that the structure of the tonoplast was damaged by this treatment. Further support for this conclusion comes from results showing that the concentration of thiosulfinates [which are produced only by catalytic conversion of S-alk(en)yl-l-cysteine sulfoxides in cytosol by alliinase located in the vacuole] in the acetic acid pickling solution is 1.3 mg/mL, but almost no thiosulfinates were detected in the pickling solution of citric and malic acids. Thus, all present results suggest that damage of tonoplast by treatment with monocarboxylates such as acetic acid may be the main reason for the greening of garlic.     

Normal phase liquid chromatographic determination of sulfamethoxazole in tablets: collaborative study

A stability-indicating liquid chromatographic method is presented for determining sulfamethoxazole in tablets. The method uses a 10 micron silica column, an isooctane-methylene chloride-2-propanol-acetonitrile-glacial acetic acid (70 + 25 + 5 + 5 + 0.5) mobile phase, and photometric detection at 254 nm. Seven laboratories collaboratively studied this method on powdered composite samples prepared from commercial 500 and 1000 mg tablets and on an authentic tablet mixture containing 83.32% added sulfamethoxazole. Mean assay results for the 500 and 1000 mg tablets were 102.2 and 97.9% of declared, respectively (n = 4). The mean recovery value for the synthetic sample was 99.4% (n = 4). The pooled reproducibility standard deviation (SD) (coefficient of variation (CV)) and pooled repeatability SD (CV) were +/- 1.01 (1.01%) and +/- 0.96 (0.96%), respectively. These results were in good agreement with those obtained by the Associate Referee for the titration method of USP XX. The proposed method can also be used for monitoring the presence of sulfanilamide in sulfamethoxazole by increasing the proportions of both acetonitrile and 2-propanol in the mobile phase. The method has been adopted official first action.     

Comparison of Low-Molecular-Weight Organic Acids and Ethylenediaminetetraacetic Acid to Enhance Phytoextraction of Heavy Metals by Maize

We compared acetic, ascorbic, and oxalic acids with ethylenediaminetetraacetic acid (EDTA) to enhance phytoextraction of nickel (Ni), manganese (Mn), zinc (Zn), copper (Cu), cadmium (Cd), and lead (Pb) by maize. Except ascorbic acid, acids significantly (P < 0.05) decreased shoot dry weight with maximum (5.60 g pot^?1) recorded with ascorbic acid and minimum with oxalic acid (4.06 g pot^?1). Maximum ammonium bicarbonate–diethylenetriaminepenta acetic acid (AB-DTPA)–extractable nickel (19.94 mg kg^?1) was recorded with EDTA and it was minimum (10.57 mg kg^?1) with oxalic acid. The EDTA significantly (P < 0.05) increased AB-DTPA-extractable lead while other acids decreased it. Except acetic acid, other acids significantly (P < 0.05) increased Ni and Zn concentration in shoots with maximum Ni (9.22 mg kg^?1) and Zn (37.40 mg kg^?1) with EDTA.     

Collaborative study of a spectrophotometric method for determining maleic hydrazide residues in tobacco and vegetables.

A distillation-spectrophotometric method for the determination of maleic hydrazide residues in tobacco and vegetables reported previously was studied collaboratively. Ten laboratories submitted analytical results on 10 samples containing residues resulting either from field treatment or laboratory fortification. The samples were estimated to contain from 0.99 to 16.36 mug maleic hydrazide/0.5 g sample analyzed. The coefficients of variation based on precision standard deviation ranged from 57.7% for the lowest residue content to 32.4% for the highest. The corresponding coefficients of variation based on overall standard deviations were estimated to be at least one-fifth larger. Strong evidence of systematic laboratory differences was found (F-test, significant at 0.1%). Apparent recoveries of 10.0 mug maleic hydrazide added to 0.5 g fluecured tobacco and potato were 97.3 and 89.7%, respectively. Apparent recoveries of 16.0 and 16.5 mug added to 0.5 g green bean were 87.4 and 85.5%, respectively. The precision of the method studied was no better than that of the current official final action method, 29.121--29.127, and its adoption is not recommended.     

Comparison of Analytical Methods for Quantifying the Levels of Lead,Cadmium, Chromium,and Nickel in Mineral Fertilizers and Industrial By-products

The control of contaminants in fertilizers and industrial by-products is fundamental to safe food production, and it requires low-cost, reliable test methods. The aim of this study was to evaluate the performance of the USEPA 3051a and alternative analytical methods [concentrated hydrochloric acid (HCl), 10 percent HCl, 10 percent sulfuric acid (H₂SO₄), and 50 mmol L^?1 diethylenetriaminepentaacetic acid (DTPA)] for quantifying the levels of lead, cadmium, chromium, and nickel in zinc and/or copper sources. The sample digestions with concentrated HCl, H₂SO₄, and nitric acid (HNO₃) (USEPA 3051a) were heated. Extraction without heating and stirring was employed in 10 percent HCl and 50 mmol L^?1 DTPA methods. The Graybill’s modified F-test, t-test for mean error, and the linear correlation coefficient analysis were used to compare test method performance. Equivalent results to USEPA 3051a were found with the following methods: DTPA for the extraction of lead in zinc sources and concentrated HCl and H₂SO₄ for the extraction of cadmium and chromium in copper sources. However, the absolute values of cadmium, chromium, and nickel recovered by the use of H₂SO₄ were greater regardless of the source. The greater extraction of contaminants in the evaluated methods suggests that there is need to review the official method if the aim is to quantify the total levels of these elements in raw materials and mineral fertilizers.     

Gas chromatographic determination of pentachlorophenol in gelatin: collaborative study

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.     

腐殖酸对池塘底泥中铅、镉的离子形态分布及其活性的影响

本文探讨了腐殖酸对池塘底泥中铅、镉的离子形态分布及其活性的影响。结果表明,富里酸(FA)能使底泥中铅、镉的碳酸盐结合态、铁锰氧化物结合态和残渣态的含量下降,而有机结合态和可溶态的含量升高,但是胡敏酸(HA)则使其它各形态均向有机结合态转化。随着FA浓度的提高底泥中铅、镉的可溶态含量也呈增高的趋势,但是HA的作用与此相反,这就表明FA能活化底泥中的铅、镉,而HA则起到了钝化作用,且它们的作用随着浓度的增大而增大。另外,无论是FA还是HA它们对底泥中铅、镉的离子形态分布及其活性的影响均表现出对铅的作用大于对镉的作用。     

不同土壤质地条件下麦秸、铅对镉在水稻-土壤系统中迁移的影响

通过室外砂土和黏土的大型土柱栽培试验,研究了麦秸、铅对镉在水稻-土壤中迁移的影响。研究结果表明,在砂土和黏土中随着水稻的生长发育,水稻植株镉含量逐渐降低,添加铅和麦秸均促进了水稻对镉的吸收,增加了水稻植株镉的含量,且铅的促进效应大于麦秸处理。添加铅和麦秸有利于镉向籽粒的转运和提高水稻籽粒镉的富集系数,砂土中添加铅、麦秸的处理籽粒镉含量和富集系数比镉单一处理分别增加44.00%、36.00%和41.67%、50.00%;黏土中分别增加58.62%、43.00%和46.15%、61.54%。镉进入土壤后会随着水分流动向下迁移,在砂土中的迁移能力大于黏土。随着土壤深度的增加镉含量逐渐减少,黏土在40～60cm、砂土在60～80cm土层中镉含量与对照含量差异不显著。添加铅和麦秸可以降低镉在土壤中向下迁移的能力,降低幅度黏土大于砂土。     

Reverse-phase liquid chromatographic determination of dexamethasone acetate and cortisone acetate in bulk drug substance and dosage forms: collaborative study

A reverse-phase liquid chromatographic method for determination of dexamethasone acetate and of cortisone acetate was subjected to an interlaboratory study by 8 collaborators for each steroid acetate. Bulk drug substance, suspensions, and tablets were assayed. Bulk drug or dosage form is dissolved in an acetonitrile-buffer mixture and analyzed by an external standard method. The steroid acetate is resolved from extraneous components by reverse-phase chromatography and detected at 254 nm. The sample solutions are stable for at least 72 h. For dexamethasone acetate, coefficients of variation were 0.9 and less than or equal to 3.1% for the bulk drug substance and the suspensions, respectively. For cortisone acetate, coefficients of variation were 0.7% for bulk material, less than or equal to 2.0% for suspensions, and less than or equal to 2.5% for tablets. All dosage forms were commercial formulations. The 2 methods have been adopted official first action.