Journal - Association of Official Analytical Chemists最新文献

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Analysis of organochlorine pesticide residues using simultaneous injection of two capillary columns with electron capture and electrolytic conductivity detectors. 电子捕获电导检测器双毛细管柱同时进样分析有机氯农药残留。
M L Hopper
{"title":"Analysis of organochlorine pesticide residues using simultaneous injection of two capillary columns with electron capture and electrolytic conductivity detectors.","authors":"M L Hopper","doi":"","DOIUrl":"","url":null,"abstract":"<p><p>A system has been developed that will allow low level screening of 31 organochlorine pesticide residues using simultaneous injection on 2 dissimilar capillary columns. An electron capture detector was attached to a DB-1701 column, and an electrolytic conductivity detector in the halogen mode was attached to a DB-5 column. Chlorinated pesticide amounts ranging from 0.05 ng for gamma-BHC to 1.5 ng for decamethrin can easily be quantitated and confirmed. The system can be used in either the column programmed mode or the isothermal column mode. Good reproducibility was obtained for injections in both modes. This system can easily be retrofitted to any gas chromatograph using on column or split/splitless injectors.</p>","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"74 6","pages":"974-81"},"PeriodicalIF":0.0,"publicationDate":"1991-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"12920242","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
Assay of oxolinic acid residues in salmon muscle by liquid chromatography with fluorescence detection: interlaboratory study. 荧光液相色谱法测定鲑鱼肌肉中氧喹啉酸残留量:实验室间研究。
G Carignan, L Larocque, S Sved
{"title":"Assay of oxolinic acid residues in salmon muscle by liquid chromatography with fluorescence detection: interlaboratory study.","authors":"G Carignan,&nbsp;L Larocque,&nbsp;S Sved","doi":"","DOIUrl":"","url":null,"abstract":"<p><p>A previously developed method that uses a simplified sample preparation and fluorometric detection of liquid chromatographic eluates for the determination of oxolinic acid in salmon muscle has been collaboratively studied. Five laboratories participated in the study to analyze, in quintuplicate, blank salmon muscle fortified at 10, 20, 50, and 100 micrograms/kg (ppb), and 2 incurred samples from salmon given feed with medicated oxolinic acid. The tissue, 2 g mixed with 2 g Na2SO4, is extracted with ethyl acetate and centrifuged, and the solvent is evaporated. The residue is partitioned in a mixture of hexane and 0.01 M oxalic acid, and the aqueous phase is chromatographed using fluorescence detection at 327 nm excitation and 369 nm emission. Mean recoveries ranged from 77.2 to 84.5% in spiked samples with reproducibility relative standard deviation (RSDR) ranging from 11.5 to 18.3%. Treated salmon were found to contain 8.71 and 53.8 micrograms/kg with RSDR of 18.6 and 16.7%, respectively. The corresponding repeatability relative standard deviations (RSDR) were 5.8-12.2%, and 7.7 and 6.2%. The method is recommended for regulatory purposes in Canada.</p>","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"74 6","pages":"906-9"},"PeriodicalIF":0.0,"publicationDate":"1991-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"12920992","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
Enzymatic determination of free glutamic acid in dried soups and in minced sausages: NMKL collaborative study. 酶法测定干汤和碎香肠中游离谷氨酸:NMKL合作研究。
Journal - Association of Official Analytical Chemists Pub Date : 1991-11-01 DOI: 10.1093/JAOAC/74.6.921
M. Hattula, H. Wallin
{"title":"Enzymatic determination of free glutamic acid in dried soups and in minced sausages: NMKL collaborative study.","authors":"M. Hattula, H. Wallin","doi":"10.1093/JAOAC/74.6.921","DOIUrl":"https://doi.org/10.1093/JAOAC/74.6.921","url":null,"abstract":"An enzymatic method for the determination of free glutamic acid in meat products and dried soups was collaboratively studied in 11 laboratories. In the presence of the enzyme glutamate dehydrogenase, L-glutamic acid is oxidatively deaminated by nicotinamide adenine dinucleotide (NAD) to 2-oxoglutarate. In a reaction catalyzed by diaphorase, the NADH thus formed converts 2-(p-iodophenyl)-3-(p-nitrophenyl)-5-phenyltetrazolium chloride to a formazan, which is measured in the visible range at 492 nm. Fourteen samples (7 samples of minced sausage and 7 samples of dried cauliflower soup) with glutamate contents varying between 0.4 and 16 g/kg were included in the study. Materials were distributed to participants as blind duplicates and as split level pairs. The mean relative standard deviation (RSDR) for reproducibility for the dried soup material containing glutamate between 7 and 16 g/kg was 4.6%. RSDR values for samples of minced sausage containing glutamate at lower levels (0.4-1.3 g/kg) were between 12 and 16%.","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"10 1","pages":"921-5"},"PeriodicalIF":0.0,"publicationDate":"1991-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"90823366","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: 3
Liquid chromatographic determination of paralytic shellfish poisons in shellfish after prechromatographic oxidation. 色谱前氧化贝类中麻痹性贝类毒素的液相色谱测定。
Journal - Association of Official Analytical Chemists Pub Date : 1991-11-01 DOI: 10.1093/JAOAC/74.6.1006
J. F. Lawrence, C. Ménard
{"title":"Liquid chromatographic determination of paralytic shellfish poisons in shellfish after prechromatographic oxidation.","authors":"J. F. Lawrence, C. Ménard","doi":"10.1093/JAOAC/74.6.1006","DOIUrl":"https://doi.org/10.1093/JAOAC/74.6.1006","url":null,"abstract":"A liquid chromatographic method for quantitating paralytic shellfish poison toxins in shellfish has been developed in which the toxins are converted to fluorescent purines by prechromatographic oxidation under mildly basic conditions with hydrogen peroxide or periodate. The addition of ammonium formate to the periodate oxidation reaction greatly improved the yield of fluorescent derivatives for neosaxitoxin, gonyautoxin-1, B-2, and C-3 compared to the same reaction without ammonium formate. As little as 3-6 ng of each of the nonhydroxylated toxins and 7-12 ng of the hydroxylated compounds per gram of shellfish could be detected. Reversed-phase chromatography using ammonium formate in the mobile phase improved the chromatography of neosaxitoxin and B-2 compared to results obtained earlier. Because the oxidation products of neosaxitoxin and B-2 could not be separated, parent compounds were separated before oxidation by using an SPE-COOH ion exchange cartridge. The repeatability coefficient of variation for the oxidation reactions ranged from 3 to 8% for the peroxide reaction, and from 4 to 11% for the periodate reaction, depending upon the individual toxin determined and its concentration in the extract (0.04-0.55 micrograms/g). The method was compared to the mouse bioassay and the postcolumn oxidation method. In most cases, results were comparable.","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"19 1","pages":"1006-12"},"PeriodicalIF":0.0,"publicationDate":"1991-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76941892","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: 72
Use of the Mycosep multifunctional cleanup column for liquid chromatographic determination of aflatoxins in agricultural products. 应用Mycosep多功能净化柱液相色谱法测定农产品中黄曲霉毒素。
T J Wilson, T R Romer
{"title":"Use of the Mycosep multifunctional cleanup column for liquid chromatographic determination of aflatoxins in agricultural products.","authors":"T J Wilson,&nbsp;T R Romer","doi":"","DOIUrl":"","url":null,"abstract":"<p><p>A liquid chromatographic (LC) technique has been developed that uses the Mycosep multifunctional cleanup (MFC) column. MFC columns provide a rapid 1-step extract purification. They are designed to retain particular groups of compounds that may create interferences in analytical methods. At the same time, MFC columns allow compounds of interest to pass through. In the method presented, test samples are extracted in a blender with acetonitrile-water (9 + 1). A portion of the extract is forced through an MFC column designed especially for analysis of numerous mycotoxins. Analytical interferences are retained, while aflatoxins pass through the column. Aflatoxins B1 and G1 are converted to their hemiacetals by heating a mixture of purified extract and water-trifluoroacetic acid-acetic acid (7 + 2 + 1) at 65 degrees C for 8.5 min. An aliquot of this mixture is analyzed by isocratic LC with acetonitrile-water mobile phase and fluorescence detection. A detection limit of less than 0.5 ng/g for aflatoxin B1 was obtained. Average recoveries greater than 95% total aflatoxins (B1, B2, G1, and G2) and coefficients of variation of less than 3% were obtained. The method was successfully applied to the following commodities: corn, almonds, pista-chios, walnuts, peanuts, Brazil nuts, milo, rice, cottonseed, corn meal, corn gluten meal, fig paste, and mixed feeds.</p>","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"74 6","pages":"951-6"},"PeriodicalIF":0.0,"publicationDate":"1991-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"12920236","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
Supercritical fluid extraction/enzyme assay: a novel technique to screen for pesticide residues in meat products. 超临界流体萃取/酶分析:一种筛选肉制品中农药残留的新技术。
J E France, J W King
{"title":"Supercritical fluid extraction/enzyme assay: a novel technique to screen for pesticide residues in meat products.","authors":"J E France,&nbsp;J W King","doi":"","DOIUrl":"","url":null,"abstract":"<p><p>The novel combination of supercritical fluid extraction (SFE) with an enzyme assay system has been used to screen meat products to detect the presence of pesticides. Analytes are collected in water by expanding supercritical carbon dioxide to atmospheric pressure through a restrictor and into an aqueous phase. The solution is then tested for the presence of pesticide residues by enzyme assay. Two experimental approaches have been used. Alachlor-fortified lard and bovine liver were monitored by static SFE coupled with an enzyme immunoassay. SFE of carbofuran-fortified frankfurters was coupled with an enzyme assay based on cholinesterase inhibition. A major benefit of the SFE/enzyme assay technique over conventional screening techniques is that the analyst is not exposed to organic solvents.</p>","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"74 6","pages":"1013-6"},"PeriodicalIF":0.0,"publicationDate":"1991-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"12920990","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
Identification of whale species by thin-layer isoelectric focusing of sarcoplasmic proteins. 用肌浆蛋白薄层等电聚焦法鉴定鲸鱼种类。
Journal - Association of Official Analytical Chemists Pub Date : 1991-11-01 DOI: 10.1093/JAOAC/74.6.943
Y. Ukishima, M. Kino, H. Kubota, S. Wada, S. Okada
{"title":"Identification of whale species by thin-layer isoelectric focusing of sarcoplasmic proteins.","authors":"Y. Ukishima, M. Kino, H. Kubota, S. Wada, S. Okada","doi":"10.1093/JAOAC/74.6.943","DOIUrl":"https://doi.org/10.1093/JAOAC/74.6.943","url":null,"abstract":"Thin-layer isoelectric focusing was applied to the identification of whale (Cetacea) species by using water-soluble sarcoplasmic proteins of skeletal muscles. Twenty-eight samples consisting of 4 species (10 samples) of baleen whales (Mysticeti) and 8 species (18 samples) of toothed whales (Odontoceti) were analyzed. Each sample (approximately 1 g) was electrophoresed with Ampholine PAGplate, pH 3.5-9.5. The electrophoretic profiles were species-specific on the 4 toothed whale species that did not have a marked intra-species difference, and all 4 baleen whale species. However, the profiles were not specific on the 4 other dolphin species, even though they were discriminable from the other 4 toothed whale species. Numerical values of pIs and relative peak heights were obtained by densitometric analysis of the isoelectro-focused protein bands. The bands were also species-specific for the 8 toothed whale species mentioned. The values may be applicable to species identification without the need for a standard sample, which may not be readily obtainable. Experiments on test samples of minke and sel whales showed that bloodletting with ice water made the densities of isoelectro-focused bands thinner, although species identification was still possible by using the inside part of muscles. Heat treatment at below 60 degrees C for 10 min caused little denaturation; at higher temperatures the protein bands were diminished in a temperature-dependent fashion. Therefore, the present isoelectric focusing analysis should be applicable to small samples of whale meat, excluding several species of dolphins.","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"48 1","pages":"943-50"},"PeriodicalIF":0.0,"publicationDate":"1991-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"89975916","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
Analysis of trypsin inhibitors and lectins in white kidney beans (Phaseolus vulgaris, var. Processor) in a combined method. 联合方法分析白芸豆(Phaseolus vulgaris, var. Processor)中胰蛋白酶抑制剂和凝集素。
J P Roozen, J de Groot
{"title":"Analysis of trypsin inhibitors and lectins in white kidney beans (Phaseolus vulgaris, var. Processor) in a combined method.","authors":"J P Roozen,&nbsp;J de Groot","doi":"","DOIUrl":"","url":null,"abstract":"<p><p>Buffered saline extraction, affinity chromatography, and Folin-BSA protein assay were used consecutively to provide a combined method for analysis of trypsin inhibitors and lectins in white kidney beans (Phaseolus vulgaris, var. Processor). The method was tested by following the decrease of both antinutritional factors by germination of the beans for 7 days at 20 degrees C. Repeatability coefficients of variation were 2-7.4% for the trypsin inhibitors and 2.2-10% for the lectins. After 7 days of germination, trypsin inhibitors and lectins were reduced by 72 and 92%, respectively.</p>","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"74 6","pages":"940-3"},"PeriodicalIF":0.0,"publicationDate":"1991-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"12920240","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
Polyvinyl chloride matrix membrane electrodes for manual and flow injection analysis of chloroquine in pharmaceutical preparations. 用于药物制剂中氯喹手工和流动注射分析的聚氯乙烯基质膜电极。
S S Hassan, M A Ahmed
{"title":"Polyvinyl chloride matrix membrane electrodes for manual and flow injection analysis of chloroquine in pharmaceutical preparations.","authors":"S S Hassan,&nbsp;M A Ahmed","doi":"","DOIUrl":"","url":null,"abstract":"<p><p>Two types of polyvinyl chloride (PVC) matrix membrane electrodes responsive to the antimalarial drug chloroquine have been constructed, electrochemically evaluated, compared and used in pharmaceutical analysis. Type 1 is the classic PVC model with chloroquine-tetraphenylborate (TPB) sensor; Type 2 is a coated silver disk without internal filling solution. Both electrode types exhibited rapid linear potentiometric response to the logarithmic concentration of diprotonated chloroquine cation in the 10(-1) - 10(-6)M range with calibration slopes 28-30 mV/concentration decade over the pH range 1.8-6.2. These electrodes were sensitive enough to permit determination of chloroquine phosphate at concentrations as low as 5 microgram/mL with good accuracy and precision. Determination of chloroquine in various pharmaceutical preparations using direct potentiometry and potentiometric titration with NaTPB gave an average recovery of 98.8% of the nominal values (SD 0.5%). The Type 2 electrode was also assessed in a flow-through sandwich cell for flow injection analysis. Results were compared with data obtained by the U.S. Pharmacopeia method.</p>","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"74 6","pages":"900-5"},"PeriodicalIF":0.0,"publicationDate":"1991-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"12920988","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
Identification of whale species by thin-layer isoelectric focusing of sarcoplasmic proteins. 用肌浆蛋白薄层等电聚焦法鉴定鲸鱼种类。
Y Ukishima, M Kino, H Kubota, S Wada, S Okada
{"title":"Identification of whale species by thin-layer isoelectric focusing of sarcoplasmic proteins.","authors":"Y Ukishima,&nbsp;M Kino,&nbsp;H Kubota,&nbsp;S Wada,&nbsp;S Okada","doi":"","DOIUrl":"","url":null,"abstract":"<p><p>Thin-layer isoelectric focusing was applied to the identification of whale (Cetacea) species by using water-soluble sarcoplasmic proteins of skeletal muscles. Twenty-eight samples consisting of 4 species (10 samples) of baleen whales (Mysticeti) and 8 species (18 samples) of toothed whales (Odontoceti) were analyzed. Each sample (approximately 1 g) was electrophoresed with Ampholine PAGplate, pH 3.5-9.5. The electrophoretic profiles were species-specific on the 4 toothed whale species that did not have a marked intra-species difference, and all 4 baleen whale species. However, the profiles were not specific on the 4 other dolphin species, even though they were discriminable from the other 4 toothed whale species. Numerical values of pIs and relative peak heights were obtained by densitometric analysis of the isoelectro-focused protein bands. The bands were also species-specific for the 8 toothed whale species mentioned. The values may be applicable to species identification without the need for a standard sample, which may not be readily obtainable. Experiments on test samples of minke and sel whales showed that bloodletting with ice water made the densities of isoelectro-focused bands thinner, although species identification was still possible by using the inside part of muscles. Heat treatment at below 60 degrees C for 10 min caused little denaturation; at higher temperatures the protein bands were diminished in a temperature-dependent fashion. Therefore, the present isoelectric focusing analysis should be applicable to small samples of whale meat, excluding several species of dolphins.</p>","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"74 6","pages":"943-50"},"PeriodicalIF":0.0,"publicationDate":"1991-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"12920995","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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