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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
M T Hattula, H C Wallin
{"title":"Enzymatic determination of free glutamic acid in dried soups and in minced sausages: NMKL collaborative study.","authors":"M T Hattula,&nbsp;H C Wallin","doi":"","DOIUrl":"","url":null,"abstract":"<p><p>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%.</p>","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"74 6","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":"12848805","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
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。
Journal - Association of Official Analytical Chemists Pub Date : 1991-11-01 DOI: 10.1093/JAOAC/74.6.940
J. 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. Roozen, J. de Groot","doi":"10.1093/JAOAC/74.6.940","DOIUrl":"https://doi.org/10.1093/JAOAC/74.6.940","url":null,"abstract":"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.","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"58 1","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":"85228597","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: 7
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。
Journal - Association of Official Analytical Chemists Pub Date : 1991-11-01 DOI: 10.1093/JAOAC/74.6.900
S. Hassan, M. Ahmed
{"title":"Polyvinyl chloride matrix membrane electrodes for manual and flow injection analysis of chloroquine in pharmaceutical preparations.","authors":"S. Hassan, M. Ahmed","doi":"10.1093/JAOAC/74.6.900","DOIUrl":"https://doi.org/10.1093/JAOAC/74.6.900","url":null,"abstract":"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.","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"26 1","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":"83132321","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 paraquat and diquat in crops using a silica column with aqueous ionic mobile phase. 水离子流动相硅柱液相色谱法测定作物中百草枯和双菊枯。
Journal - Association of Official Analytical Chemists Pub Date : 1991-11-01 DOI: 10.1093/JAOAC/74.6.961
T. M. Chichila, S. M. Walters
{"title":"Liquid chromatographic determination of paraquat and diquat in crops using a silica column with aqueous ionic mobile phase.","authors":"T. M. Chichila, S. M. Walters","doi":"10.1093/JAOAC/74.6.961","DOIUrl":"https://doi.org/10.1093/JAOAC/74.6.961","url":null,"abstract":"A method was developed for the determination of paraquat (PQ) and diquat (DQ) in high moisture food crops. Samples were digested with 6M HCl, and the herbicides were isolated from the digest using pH-controlled silica solid phase extraction. The analytes were then determined by ion-pairing liquid chromatography with a silica analytical column, sodium chloride as the ion-pairing reagent, and acetonitrile as the organic modifier. A diode array UV absorbance detector was used to simultaneously quantify PQ and DQ at their respective maximum absorbance wavelengths, 257 and 310 nm. Average recoveries of PQ and DQ standards from 4 different crops fortified at 0.01-0.50 ppm levels ranged from 79.3 to 104.8%.","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"186 1","pages":"961-7"},"PeriodicalIF":0.0,"publicationDate":"1991-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"86092540","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
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。
Journal - Association of Official Analytical Chemists Pub Date : 1991-11-01 DOI: 10.1093/JAOAC/74.6.951
Thomas J Wilson, T. Romer
{"title":"Use of the Mycosep multifunctional cleanup column for liquid chromatographic determination of aflatoxins in agricultural products.","authors":"Thomas J Wilson, T. Romer","doi":"10.1093/JAOAC/74.6.951","DOIUrl":"https://doi.org/10.1093/JAOAC/74.6.951","url":null,"abstract":"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.","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"17 1","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":"75273626","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: 50
Limited survey of residual tetracyclines in tissues collected from diseased animals in Aichi Prefecture, Japan. 日本爱知县患病动物组织中残留四环素的有限调查。
Journal - Association of Official Analytical Chemists Pub Date : 1991-11-01
H Oka, Y Ikai, N Kawamura, J Hayakawa
{"title":"Limited survey of residual tetracyclines in tissues collected from diseased animals in Aichi Prefecture, Japan.","authors":"H Oka,&nbsp;Y Ikai,&nbsp;N Kawamura,&nbsp;J Hayakawa","doi":"","DOIUrl":"","url":null,"abstract":"<p><p>Tissues were collected to survey the actual conditions of tetracycline antibiotics (TCs) residues in slaughtered animals that did not pass inspection at slaughterhouses in Aichi Prefecture, Japan, because of the presence of disease symptoms. Tissues were analyzed by liquid chromatography. Among 271 samples, 49 (18.1%) were positive for oxytetracycline (OTC), 5 (1.8%) for chlortetracycline (CTC), and 5 (1.8%) for doxycycline (DC), respectively. One sample (cattle kidney) was positive for both OTC and DC. However, tetracycline was not detected in any samples. Percentage frequencies of TCs residues were 29.1% (37/127) and 15.2% (22/144) for cattle and hogs, respectively. Kidney samples showed higher incidence of TCs residues and 1.5-7 times higher residual concentrations than liver and miscellaneous samples.</p>","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"74 6","pages":"894-6"},"PeriodicalIF":0.0,"publicationDate":"1991-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"12920451","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
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。
Journal - Association of Official Analytical Chemists Pub Date : 1991-11-01 DOI: 10.1093/JAOAC/74.6.974
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":"10.1093/JAOAC/74.6.974","DOIUrl":"https://doi.org/10.1093/JAOAC/74.6.974","url":null,"abstract":"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.","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"1 1","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":"76785059","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
Liquid chromatographic determination of the processing aid 4-hexylresorcinol in shrimp. 虾中加工助剂4-己基间苯二酚的液相色谱测定。
Journal - Association of Official Analytical Chemists Pub Date : 1991-11-01 DOI: 10.1093/JAOAC/74.6.1003
J. M. King, A. J. Mcevily, R. Iyengar
{"title":"Liquid chromatographic determination of the processing aid 4-hexylresorcinol in shrimp.","authors":"J. M. King, A. J. Mcevily, R. Iyengar","doi":"10.1093/JAOAC/74.6.1003","DOIUrl":"https://doi.org/10.1093/JAOAC/74.6.1003","url":null,"abstract":"A rapid, sensitive, liquid chromatographic (LC) method has been developed for determination of residuals of the processing aid, 4-hexylresorcinol, on shrimp meat. An aqueous homogenate of shrimp meat is extracted with ethyl acetate followed by precolumn preparation on a silica Sep-Pak cartridge. LC determination is preformed with a Nova-Pak C18 column, with UV detection at 214 nm. Sensitivity was 0.006 micrograms, and recovery from shrimp meat samples of known 4-hexylresorcinol addition was 94%. Shrimp treated with 4-hexylresorcinol under the recommended dip protocol had mean residuals of 1.18 ppm, with a standard deviation of 0.13 ppm.","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"71 1","pages":"1003-5"},"PeriodicalIF":0.0,"publicationDate":"1991-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"90483825","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
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。
Journal - Association of Official Analytical Chemists Pub Date : 1991-11-01 DOI: 10.1093/JAOAC/74.6.1013
J. E. France, J. King
{"title":"Supercritical fluid extraction/enzyme assay: a novel technique to screen for pesticide residues in meat products.","authors":"J. E. France, J. King","doi":"10.1093/JAOAC/74.6.1013","DOIUrl":"https://doi.org/10.1093/JAOAC/74.6.1013","url":null,"abstract":"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.","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"24 1","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":"73712619","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: 7
Liquid chromatographic determination of paraquat and diquat in crops using a silica column with aqueous ionic mobile phase. 水离子流动相硅柱液相色谱法测定作物中百草枯和双菊枯。
Journal - Association of Official Analytical Chemists Pub Date : 1991-11-01
T M Chichila, S M Walters
{"title":"Liquid chromatographic determination of paraquat and diquat in crops using a silica column with aqueous ionic mobile phase.","authors":"T M Chichila,&nbsp;S M Walters","doi":"","DOIUrl":"","url":null,"abstract":"<p><p>A method was developed for the determination of paraquat (PQ) and diquat (DQ) in high moisture food crops. Samples were digested with 6M HCl, and the herbicides were isolated from the digest using pH-controlled silica solid phase extraction. The analytes were then determined by ion-pairing liquid chromatography with a silica analytical column, sodium chloride as the ion-pairing reagent, and acetonitrile as the organic modifier. A diode array UV absorbance detector was used to simultaneously quantify PQ and DQ at their respective maximum absorbance wavelengths, 257 and 310 nm. Average recoveries of PQ and DQ standards from 4 different crops fortified at 0.01-0.50 ppm levels ranged from 79.3 to 104.8%.</p>","PeriodicalId":14752,"journal":{"name":"Journal - Association of Official Analytical Chemists","volume":"74 6","pages":"961-7"},"PeriodicalIF":0.0,"publicationDate":"1991-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"12827510","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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