D C Holland, K C Faul, J E Roybal, R K Munns, W Shimoda
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%.
{"title":"Liquid chromatographic determination of chlortetracycline hydrochloride in ruminant and poultry/swine feeds.","authors":"D C Holland, K C Faul, J E Roybal, R K Munns, W Shimoda","doi":"","DOIUrl":"","url":null,"abstract":"<p><p>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%.</p>","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"74 5","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":"12947402","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}
The precision parameters of the method-performance (collaborative) studies published in the AOAC Journal from 1915 through 1990 for pesticide formulations have been recalculated on a uniform basis by the International Union of Pure and Applied Chemistry 1987 protocol. About 93% of the 953 accepted assays, which are predominantly gravimetric (G), volumetric (V), and gas (GC) and liquid (LC) chromatographic methods, exhibit relative standard deviations among laboratories (RSDR) that are generally less than 2 times the values predicted from the Horwitz equation: RSDR (%) = 2 exp (1-0.5 log C), where C is the concentration expressed as a decimal fraction. UV, VIS, and IR spectrophotometric (S) methods are somewhat poorer, with about 80% of the reported RSDR values less than twice the predicted RSDR value. The precision parameters of pesticide formulations analyzed by the older methods (G, V, GC) are equivalent to those previously found for drug preparations in the same concentration range; the precision parameters of pesticide formulations analyzed by LC and S are somewhat poorer. Overall, however, the precision parameters of pesticide formulations are generally independent of analyte, method, and matrix, and are primarily a function of concentration. The method-acceptability decisions of the AOAC for pesticide formulations during the past 75 years can be approximated retrospectively by using a criterion for RSDR that is less than 2 times the RSDR calculated from the Horwitz equation.
{"title":"Performance characteristics of methods of analysis used for regulatory purposes. Part II. Pesticide formulations.","authors":"W. Horwitz, R. Albert","doi":"10.1093/JAOAC/74.5.718","DOIUrl":"https://doi.org/10.1093/JAOAC/74.5.718","url":null,"abstract":"The precision parameters of the method-performance (collaborative) studies published in the AOAC Journal from 1915 through 1990 for pesticide formulations have been recalculated on a uniform basis by the International Union of Pure and Applied Chemistry 1987 protocol. About 93% of the 953 accepted assays, which are predominantly gravimetric (G), volumetric (V), and gas (GC) and liquid (LC) chromatographic methods, exhibit relative standard deviations among laboratories (RSDR) that are generally less than 2 times the values predicted from the Horwitz equation: RSDR (%) = 2 exp (1-0.5 log C), where C is the concentration expressed as a decimal fraction. UV, VIS, and IR spectrophotometric (S) methods are somewhat poorer, with about 80% of the reported RSDR values less than twice the predicted RSDR value. The precision parameters of pesticide formulations analyzed by the older methods (G, V, GC) are equivalent to those previously found for drug preparations in the same concentration range; the precision parameters of pesticide formulations analyzed by LC and S are somewhat poorer. Overall, however, the precision parameters of pesticide formulations are generally independent of analyte, method, and matrix, and are primarily a function of concentration. The method-acceptability decisions of the AOAC for pesticide formulations during the past 75 years can be approximated retrospectively by using a criterion for RSDR that is less than 2 times the RSDR calculated from the Horwitz equation.","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"6 1","pages":"718-44"},"PeriodicalIF":0.0,"publicationDate":"1991-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78757530","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}
Jong P Hsu, Herbert J Schattenberg, Martha M Garza
A rapid multiresidue screen for 110 pesticides was applied to 5628 produce samples. Samples were extracted, analyzed, and evaluated within 6 1/2 h of receipt. Analyses were confirmed within a 24 h period on those samples in which a potential residue was found above the U.S. Environmental Protection Agency's tolerance level. A thorough yet quick chromatographic interpretation program is also described.
{"title":"Fast turnaround multiresidue screen for pesticides in produce.","authors":"Jong P Hsu, Herbert J Schattenberg, Martha M Garza","doi":"10.1093/JAOAC/74.5.886","DOIUrl":"https://doi.org/10.1093/JAOAC/74.5.886","url":null,"abstract":"A rapid multiresidue screen for 110 pesticides was applied to 5628 produce samples. Samples were extracted, analyzed, and evaluated within 6 1/2 h of receipt. Analyses were confirmed within a 24 h period on those samples in which a potential residue was found above the U.S. Environmental Protection Agency's tolerance level. A thorough yet quick chromatographic interpretation program is also described.","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"117 1","pages":"886-92"},"PeriodicalIF":0.0,"publicationDate":"1991-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"74288490","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}
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.
{"title":"Competitive direct enzyme-linked immunosorbent screening assay for the detection of sulfamethazine contamination of animal feeds.","authors":"D. Dixon-Holland, S. Katz","doi":"10.1093/JAOAC/74.5.784","DOIUrl":"https://doi.org/10.1093/JAOAC/74.5.784","url":null,"abstract":"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.","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"13 1","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":"80861305","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}
The homogeneity of test substances in a carrier (animal feed) is a critical factor in conducting long-term feeding studies in laboratory animals. A method for determining the adequate amount of mixing to achieve homogeneity by a mixer of the type described has been determined when 2 distinctly different compounds are added to ground dog feed. Nicotinic acid and butylated hydroxyanisole at a concentration of 1% were separately mixed with the dog feed for 15, 30, 45, 60, and 120 min to determine optimum mixing time. Test portions were taken from 4 different sampling sites at each time period and analyzed in duplicate for the added substance. Four batches were prepared and the results were aggregated. Very little interbatch variability was observed. The variance of the average values from the 4 sampling sites at each time period was calculated and used as a simple, crude, but effective numerical quantity to monitor the approach to homogeneity of the mixture.
{"title":"Time required to achieve homogeneity of test substances added to dog feed.","authors":"P P Sapienza, G J Ikeda, P I Warr, R H Albert","doi":"","DOIUrl":"","url":null,"abstract":"<p><p>The homogeneity of test substances in a carrier (animal feed) is a critical factor in conducting long-term feeding studies in laboratory animals. A method for determining the adequate amount of mixing to achieve homogeneity by a mixer of the type described has been determined when 2 distinctly different compounds are added to ground dog feed. Nicotinic acid and butylated hydroxyanisole at a concentration of 1% were separately mixed with the dog feed for 15, 30, 45, 60, and 120 min to determine optimum mixing time. Test portions were taken from 4 different sampling sites at each time period and analyzed in duplicate for the added substance. Four batches were prepared and the results were aggregated. Very little interbatch variability was observed. The variance of the average values from the 4 sampling sites at each time period was calculated and used as a simple, crude, but effective numerical quantity to monitor the approach to homogeneity of the mixture.</p>","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"74 5","pages":"857-61"},"PeriodicalIF":0.0,"publicationDate":"1991-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"12945739","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}
M P Korver, V W Burse, L L Needham, V E Green, D L Gray, M A Rouse, T L Shelly, B K Mortensen
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.
{"title":"Determination of Mirex in human blood serum containing polychlorinated biphenyls by using packed column gas chromatography.","authors":"M P Korver, V W Burse, L L Needham, V E Green, D L Gray, M A Rouse, T L Shelly, B K Mortensen","doi":"","DOIUrl":"","url":null,"abstract":"<p><p>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.</p>","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"74 5","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":"12945743","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}
A rapid multiresidue screen for 110 pesticides was applied to 5628 produce samples. Samples were extracted, analyzed, and evaluated within 6 1/2 h of receipt. Analyses were confirmed within a 24 h period on those samples in which a potential residue was found above the U.S. Environmental Protection Agency's tolerance level. A thorough yet quick chromatographic interpretation program is also described.
{"title":"Fast turnaround multiresidue screen for pesticides in produce.","authors":"J P Hsu, H J Schattenberg, M M Garza","doi":"","DOIUrl":"","url":null,"abstract":"<p><p>A rapid multiresidue screen for 110 pesticides was applied to 5628 produce samples. Samples were extracted, analyzed, and evaluated within 6 1/2 h of receipt. Analyses were confirmed within a 24 h period on those samples in which a potential residue was found above the U.S. Environmental Protection Agency's tolerance level. A thorough yet quick chromatographic interpretation program is also described.</p>","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"74 5","pages":"886-92"},"PeriodicalIF":0.0,"publicationDate":"1991-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"12945744","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}
The homogeneity of test substances in a carrier (animal feed) is a critical factor in conducting long-term feeding studies in laboratory animals. A method for determining the adequate amount of mixing to achieve homogeneity by a mixer of the type described has been determined when 2 distinctly different compounds are added to ground dog feed. Nicotinic acid and butylated hydroxyanisole at a concentration of 1% were separately mixed with the dog feed for 15, 30, 45, 60, and 120 min to determine optimum mixing time. Test portions were taken from 4 different sampling sites at each time period and analyzed in duplicate for the added substance. Four batches were prepared and the results were aggregated. Very little interbatch variability was observed. The variance of the average values from the 4 sampling sites at each time period was calculated and used as a simple, crude, but effective numerical quantity to monitor the approach to homogeneity of the mixture.
{"title":"Time required to achieve homogeneity of test substances added to dog feed.","authors":"P. Sapienza, G. Ikeda, P. Warr, R. H. Albert","doi":"10.1093/JAOAC/74.5.857","DOIUrl":"https://doi.org/10.1093/JAOAC/74.5.857","url":null,"abstract":"The homogeneity of test substances in a carrier (animal feed) is a critical factor in conducting long-term feeding studies in laboratory animals. A method for determining the adequate amount of mixing to achieve homogeneity by a mixer of the type described has been determined when 2 distinctly different compounds are added to ground dog feed. Nicotinic acid and butylated hydroxyanisole at a concentration of 1% were separately mixed with the dog feed for 15, 30, 45, 60, and 120 min to determine optimum mixing time. Test portions were taken from 4 different sampling sites at each time period and analyzed in duplicate for the added substance. Four batches were prepared and the results were aggregated. Very little interbatch variability was observed. The variance of the average values from the 4 sampling sites at each time period was calculated and used as a simple, crude, but effective numerical quantity to monitor the approach to homogeneity of the mixture.","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"97 1","pages":"857-61"},"PeriodicalIF":0.0,"publicationDate":"1991-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76012875","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}
Results are compared for the microbiological analysis of chlortetracycline using the AOAC method and a modified method applicable to potencies above 50 g/ton. Two modifications are presented: substitution of a pH range of 4.0-4.5 instead of the specified pH of 4.5 for the plating solution, and substitution of extraction by shaking instead of the blending procedure. There were no significant differences in results between the AOAC method and the modified method.
{"title":"Modifications to the official method for testing chlortetracycline HCl in animal feeds.","authors":"M. L. Hasselberger","doi":"10.1093/JAOAC/74.5.790","DOIUrl":"https://doi.org/10.1093/JAOAC/74.5.790","url":null,"abstract":"Results are compared for the microbiological analysis of chlortetracycline using the AOAC method and a modified method applicable to potencies above 50 g/ton. Two modifications are presented: substitution of a pH range of 4.0-4.5 instead of the specified pH of 4.5 for the plating solution, and substitution of extraction by shaking instead of the blending procedure. There were no significant differences in results between the AOAC method and the modified method.","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"45 1","pages":"790-2"},"PeriodicalIF":0.0,"publicationDate":"1991-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77543531","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}
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.
{"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, S. M. Walters","doi":"10.1093/JAOAC/74.5.830","DOIUrl":"https://doi.org/10.1093/JAOAC/74.5.830","url":null,"abstract":"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.","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"91 1","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":"81605999","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}
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