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Bacillus stearothermophilus disk assay for determining ampicillin residues in fish muscle. 鱼肌肉中氨苄西林残留量测定的嗜热脂肪芽孢杆菌圆盘试验。
Journal - Association of Official Analytical Chemists Pub Date : 1991-11-01 DOI: 10.1093/JAOAC/74.6.910
S. M. Plakas, A. DePaola, M. Moxey
{"title":"Bacillus stearothermophilus disk assay for determining ampicillin residues in fish muscle.","authors":"S. M. Plakas, A. DePaola, M. Moxey","doi":"10.1093/JAOAC/74.6.910","DOIUrl":"https://doi.org/10.1093/JAOAC/74.6.910","url":null,"abstract":"The Bacillus stearothermophilus disk assay for penicillin in milk (AOAC official method) was adapted for the determination of ampicillin in fish muscle. The method was evaluated in 2 species of cultured fish: channel catfish and striped bass. Recoveries of ampicillin ranged from 99 to 104% when muscle specimens from both species were spiked at concentrations of 0.025-1.00 micrograms/g. The lower limit of determination (LOD) was 0.025 micrograms/g. The assay was applied to monitor the elimination of ampicillin from the muscle of striped bass after intravascular administration (dosage of 10 mg/kg body weight). The mean concentrations in the muscle declined from 1.160 micrograms/g at 2 h to 0.063 micrograms/g at 18 h. The half-life of ampicillin in the muscle was 3.6 h. Ampicillin concentrations were below LOD at 24 h. No inhibitory activity was observed in the muscle of control fish.","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"44 1","pages":"910-2"},"PeriodicalIF":0.0,"publicationDate":"1991-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"75774720","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 5
An analytical survey of aflatoxins in tissues from swine grown in regions reporting 1988 aflatoxin-contaminated corn. 1988年玉米受黄曲霉毒素污染地区猪组织中黄曲霉毒素的分析调查。
Journal - Association of Official Analytical Chemists Pub Date : 1991-11-01 DOI: 10.1093/JAOAC/74.6.897
R. Stubblefield, J. P. Honstead, O. Shotwell
{"title":"An analytical survey of aflatoxins in tissues from swine grown in regions reporting 1988 aflatoxin-contaminated corn.","authors":"R. Stubblefield, J. P. Honstead, O. Shotwell","doi":"10.1093/JAOAC/74.6.897","DOIUrl":"https://doi.org/10.1093/JAOAC/74.6.897","url":null,"abstract":"A joint project was undertaken by the Food Safety and Inspection Service (FSIS) and the Agriculture Research Service branches of the U.S. Department of Agriculture to determine the presence of aflatoxins in the U.S. meat supply during a drought year. In 1988, high incidences of aflatoxins occurred in corn grown in regions of the Midwest, Southeast, and South. Six states were identified as having serious aflatoxin contamination in their corn crop: Virginia, North and South Carolina, Texas, Iowa, and Illinois. Swine liver and pillars of diaphragm (muscle) tissues were sampled by federal FSIS Inspectors in plants located in these states. A worstcase sampling plan was conducted. Samples were taken in January 1989 from hogs fed corn soon after harvest and in April 1989 from hogs fed corn originally stored and then fed in the spring. A modification of the official AOAC method for the thin-layer chromatography (TLC) determination of aflatoxins in animal tissue was used to permit quantitation by LC with fluorescence detection. The official AOAC TLC confirmation of identity method was used to confirm all positive samples with B1 concentrations greater than 0.04 ppb and M1 concentrations greater than 0.1 ppb. Sixty samples in the January group and 100 samples in the April group were assayed. Concentrations of aflatoxins B1 and M1 in the first group of pig livers ranged from 0.04 to 0.06 ppb. The identity of aflatoxin B1 was confirmed in all positive samples. Aflatoxin M1 could not be confirmed in any of the positive liver samples because the method was insufficiently sensitive for this aflatoxin.(ABSTRACT TRUNCATED AT 250 WORDS)","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"39 6 1","pages":"897-9"},"PeriodicalIF":0.0,"publicationDate":"1991-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"85245862","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 14
Separation and determination of diesel contaminants in various fish products by capillary gas chromatography. 毛细管气相色谱法分离测定各种鱼类产品中柴油污染物。
Journal - Association of Official Analytical Chemists Pub Date : 1991-11-01 DOI: 10.1093/JAOAC/74.6.986
J. M. Newton, B. Rothman, F. Walker
{"title":"Separation and determination of diesel contaminants in various fish products by capillary gas chromatography.","authors":"J. M. Newton, B. Rothman, F. Walker","doi":"10.1093/JAOAC/74.6.986","DOIUrl":"https://doi.org/10.1093/JAOAC/74.6.986","url":null,"abstract":"A semiquantitative capillary column gas chromatographic method is described for the determination of diesel fuel contamination in various canned seafood products. The diesel contaminants are separated from the fish sample by steam distillation, with little carry-over of interfering intrinsic materials such as fish oils. The diesel fuel is extracted from the condensate with n-hexane, and the extract is analyzed on an SPB-1 fused silica capillary column. The efficiency of recovery of diesel fuel added to canned seafood at levels of 40-400 ppt ranged from 72 to 102%. With the additional step of concentrating the hexane extract, the sensitivity of this procedure may be increased at least 10-fold. This procedure can detect the differences among diesel fuel grades No. 1, 2, and 5, and variations within diesel grade No. 2, and thus may be useful in determining the type of petroleum contaminants present in various canned fish products.","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"4 1","pages":"986-90"},"PeriodicalIF":0.0,"publicationDate":"1991-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"74330458","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 4
Residue analysis of glyphosate and its principal metabolite in certain cereals, oilseeds, and pulses by liquid chromatography and postcolumn fluorescence detection. 利用液相色谱法和柱后荧光检测法对某些谷物、油籽和豆类中的草甘膦及其主要代谢物进行残留分析。
Journal - Association of Official Analytical Chemists Pub Date : 1991-09-01
Y Y Wigfield, M Lanouette
{"title":"Residue analysis of glyphosate and its principal metabolite in certain cereals, oilseeds, and pulses by liquid chromatography and postcolumn fluorescence detection.","authors":"Y Y Wigfield, M Lanouette","doi":"","DOIUrl":"","url":null,"abstract":"<p><p>A postcolumn liquid chromatographic method to determine the extractable residues of glyphosate (GLYPH) and its principal metabolite, (aminomethyl)phosphonic acid (AMPA), in various cereals and beans is described. The finely ground sample is extracted with a mixture of chloroform and water, and the resulting aqueous layer is passed through a cation exchange column. The eluate is adjusted to pH 7-10 and passed through an anion exchange column. The second column is eluted with 0.3M HCl solution and the resulting acidic eluate is analyzed with liquid chromatography coupled with postcolumn fluorescence detection. The mean recoveries for GLYPH in barley, canola, dry pea, flax, soybean, wheat, and white bean ranged from 90.0 to 98.1%, with coefficients of variation (CV) from 2.9 to 10.0% and limits of detection (LOD) from 0.07 to 0.14 ppm. Similarly, mean recoveries for AMPA in the same crops ranged from 87.4 to 98.9%, with CV from 4.6 to 7.7 and LOD from 0.05 to 0.12 ppm. Using this method, an analyst can routinely analyze 6 samples per 1.5 days. The advantages of this procedure are discussed.</p>","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"74 5","pages":"842-7"},"PeriodicalIF":0.0,"publicationDate":"1991-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"12945811","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Quantitation of the nitrosamine 2-ethylhexyl-4-(N-methyl-N-nitrosoamino) benzoate (NPABAO) in sunscreen products. 防晒产品中亚硝胺2-乙基己基-4-(n -甲基-n -亚硝基氨基)苯甲酸酯(NPABAO)的含量测定。
Journal - Association of Official Analytical Chemists Pub Date : 1991-09-01 DOI: 10.1093/JAOAC/74.5.766
T. Meyer, J. B. Powell
{"title":"Quantitation of the nitrosamine 2-ethylhexyl-4-(N-methyl-N-nitrosoamino) benzoate (NPABAO) in sunscreen products.","authors":"T. Meyer, J. B. Powell","doi":"10.1093/JAOAC/74.5.766","DOIUrl":"https://doi.org/10.1093/JAOAC/74.5.766","url":null,"abstract":"We have devised a method to quantitate the nitrosamine, 2-ethylhexyl-4-(N-methyl-N-nitrosoamino) benzoate (NPABAO), in commercial products containing the sunscreen ingredient, Padimate O. The method involves a minimum of cleanup steps to afford a nonaqueous extract from product emulsions suitable for analysis by a liquid chromatograph interfaced to a thermal energy analyzer (LC/TEA). The method is applicable to lotions, creams, and gels. Oils are normally soluble in the mobile phase and can be analyzed directly on the LC/TEA without additional cleanup procedures. The method has a minimum detectable limit of about 30 ppb and yields greater than 80% recovery. It is highly reproducible and generates no NPABAO artifactually prior to quantitation on the LC/TEA. Application of the method to 22 different commercial product formulas disclosed that the level of NPABAO in each of the products is below 250 ppb, with 18 of the products containing less than 100 ppb. Of interest was the observation that musk ketone, a common fragrance constituent, produces a false-positive TEA response that can interfere with accurate analysis of NPABAO content in typical commercial products.","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"24 1","pages":"766-71"},"PeriodicalIF":0.0,"publicationDate":"1991-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"72955938","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 2
Determination of Mirex in human blood serum containing polychlorinated biphenyls by using packed column gas chromatography. 填充柱气相色谱法测定含多氯联苯的人血清中灭雷克斯的含量。
Journal - Association of Official Analytical Chemists Pub Date : 1991-09-01 DOI: 10.1093/JAOAC/74.5.875
M. P. Korver, V. Burse, L. Needham, V. Green, D. L. Gray, M. Rouse, T. Shelly., B. Mortensen
{"title":"Determination of Mirex in human blood serum containing polychlorinated biphenyls by using packed column gas chromatography.","authors":"M. P. Korver, V. Burse, L. Needham, V. Green, D. L. Gray, M. Rouse, T. Shelly., B. Mortensen","doi":"10.1093/JAOAC/74.5.875","DOIUrl":"https://doi.org/10.1093/JAOAC/74.5.875","url":null,"abstract":"An analytical method has been developed that uses electron capture/gas-liquid chromatography to determine Mirex in serum containing polychlorinated biphenyls (PCBs) (Aroclor 1260). With this method, 0.2 ppb Mirex can be determined in 4 mL serum that also contains 10 ppb PCBs. The method provides approximately 70% recovery of Mirex at 1.0 and 3.5 ppb. The coefficients of variation are 4.5 and 4.6% at 1.0 and 3.5 ppb, respectively. In a cooperative study with the Ohio Department of Health, the Centers for Disease Control used this method to determine the extent of exposure of Salem, OH, residents to Mirex. Confirmation of Mirex was obtained by using high resolution gas chromatography and high resolution mass spectrometry.","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"31 2 1","pages":"875-7"},"PeriodicalIF":0.0,"publicationDate":"1991-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"80883493","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 2
Liquid chromatographic determination of chlortetracycline hydrochloride in ruminant and poultry/swine feeds. 反刍动物和家禽/猪饲料中盐酸氯四环素的液相色谱测定。
Journal - Association of Official Analytical Chemists Pub Date : 1991-09-01 DOI: 10.1093/JAOAC/74.5.780
D. C. Holland, K. C. Faul, J. Roybal, R. K. Munns, W. Shimoda
{"title":"Liquid chromatographic determination of chlortetracycline hydrochloride in ruminant and poultry/swine feeds.","authors":"D. C. Holland, K. C. Faul, J. Roybal, R. K. Munns, W. Shimoda","doi":"10.1093/JAOAC/74.5.780","DOIUrl":"https://doi.org/10.1093/JAOAC/74.5.780","url":null,"abstract":"A liquid chromatographic (LC) method is described for the determination of chlortetracycline hydrochloride (CTC) in poultry/swine and ruminant feeds in the 10-100 ppm range and in premix. CTC is extracted from ground feed/premix with acidified acetone, and the extract is filtered through a Millex-HV filter or disposable C18 column. The filtrate is partitioned with methylene chloride when additional cleanup is necessary. A Nova-Pak C18 column is used for LC separation with determination at 370 nm. The average recovery of CTC from premix was 95% with a standard deviation (SD) of 1.70 and a coefficient of variation (CV) of 1.79%. The overall average recovery from feeds was 77% with an SD of 3.18 and a CV of 4.10%.","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"66 1","pages":"780-4"},"PeriodicalIF":0.0,"publicationDate":"1991-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"89924843","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 8
Gas chromatographic determination of captan, folpet, and captafol residues in tomatoes, cucumbers, and apples using a wide-bore capillary column: interlaboratory study. 用宽孔毛细管柱气相色谱法测定番茄、黄瓜和苹果中上尉、上尉和上尉醇残留量:实验室间研究。
Journal - Association of Official Analytical Chemists Pub Date : 1991-09-01
D M Gilvydis, S M Walters
{"title":"Gas chromatographic determination of captan, folpet, and captafol residues in tomatoes, cucumbers, and apples using a wide-bore capillary column: interlaboratory study.","authors":"D M Gilvydis,&nbsp;S M Walters","doi":"","DOIUrl":"","url":null,"abstract":"<p><p>An interlaboratory study of the determination of captan, folpet, and captafol in tomatoes, cucumbers, and apples was conducted by 4 laboratories using wide-bore capillary column gas chromatography with electron capture detection. The 3 fungicides were determined using the Luke et al. multiresidue method modified to include additional solvent elution in the optional Florisil column cleanup step used with this method. The crops were fortified with each fungicide at 3 levels per crop. Mean recoveries ranged from 86.2% for a 25.1 ppm level of captan in apples to 115.4% for a 0.288 ppm level of captafol in apples. Interlaboratory coefficients of variation ranged from 3.4% (24.7 ppm folpet) to 9.7% (0.243 ppm captafol) for tomatoes; from 2.8% (2.0 ppm captafol) to 8.2% (24.8 ppm captan) for cucumbers; and from 1.5% (0.234 ppm folpet) to 22.1% (0.266 ppm captafol) for apples.</p>","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"74 5","pages":"830-5"},"PeriodicalIF":0.0,"publicationDate":"1991-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"12946328","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Validation of methods used in the Florida Department of Agricultural and Consumer Services' Chemical Residue Laboratory. 佛罗里达州农业和消费者服务部化学残留实验室使用的方法的验证。
Journal - Association of Official Analytical Chemists Pub Date : 1991-09-01 DOI: 10.1093/JAOAC/74.5.868
G. A. Parker
{"title":"Validation of methods used in the Florida Department of Agricultural and Consumer Services' Chemical Residue Laboratory.","authors":"G. A. Parker","doi":"10.1093/JAOAC/74.5.868","DOIUrl":"https://doi.org/10.1093/JAOAC/74.5.868","url":null,"abstract":"Very few methods for detecting residues of pesticides in food or agricultural samples have undergone rigorous colloborative study and possess official AOAC status. The Chemical Residue Laboratory has formalized a method validation scheme to use when incorporating or developing new, unofficial methods. These methods are validated by assessing certain performance parameters: scope, specificity, linear range, accuracy, precision, limit of detection (LOD), and limit of quantitation (LOQ). For accuracy and precision assessment, 12 replicate fortifications must yield recoveries within the range of 70-120% with a coefficient of variation (CV) that compares favorably to the Horwitz CV. LOD and LOQ are equivalent to 3 and 10 times, respectively, the background signal contributed by a sample matrix blank. This criterion that we use for LOD/LOQ is not universal. In fact, because of differing definitions, we have encountered difficulties in enforcing a tolerance by using a registrant's method. This paper also presents an example of our method validation scheme, using a recent method development project for detecting sulfamethazine in raw milk. The sulfamethazine project also revealed unanticipated personnel problems, underscoring the importance of the human factor in quality assurance.","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"16 1","pages":"868-71"},"PeriodicalIF":0.0,"publicationDate":"1991-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"75885566","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 17
Competitive direct enzyme-linked immunosorbent screening assay for the detection of sulfamethazine contamination of animal feeds. 竞争性直接酶联免疫吸附筛选法检测动物饲料中磺胺乙胺污染。
Journal - Association of Official Analytical Chemists Pub Date : 1991-09-01
D E Dixon-Holland, S E Katz
{"title":"Competitive direct enzyme-linked immunosorbent screening assay for the detection of sulfamethazine contamination of animal feeds.","authors":"D E Dixon-Holland,&nbsp;S E Katz","doi":"","DOIUrl":"","url":null,"abstract":"<p><p>A sensitive screening method has been developed for detecting sulfamethazine (SMZ) contamination of feeds by using either polyclonal or monoclonal antibodies and a direct competitive enzyme-linked immunosorbent screening assay (ELISA). Feed samples of 25.0 g are extracted with 0.5N HCl and centrifuged. The extract is adjusted to pH 7.0 with 3.0N NaOH and recentrifuged. This pH-adjusted extract is used in the ELISA. Levels as low as 0.004 micrograms SMZ/g feed were detected in supplemented extracts by polyclonal antibodies; levels of 0.4 micrograms SMZ/g feed were detected by a monoclonal antibody.</p>","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"74 5","pages":"784-9"},"PeriodicalIF":0.0,"publicationDate":"1991-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"12945806","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
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