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鲶鱼(斑点叉尾鮰)肌肉组织中九种氯代农药的多残留基质固相分散(MSPD)萃取及气相色谱筛查

Multiresidue matrix solid phase dispersion (MSPD) extraction and gas chromatographic screening of nine chlorinated pesticides in catfish (Ictalurus punctatus) muscle tissue.

作者信息

Long A R, Crouch M D, Barker S A

机构信息

Louisiana State University, School of Veterinary Medicine, Department of Veterinary Physiology, Pharmacology and Toxicology, Baton Rouge 70803.

出版信息

J Assoc Off Anal Chem. 1991 Jul-Aug;74(4):667-70.

PMID:1917814
Abstract

A multiresidue technique for extraction and gas chromatographic screening of 9 insecticide (lindane, heptachlor, aldrin, heptachlor epoxide, p,p'-DDE, dieldrin, endrin, p,p'-TDE, and p,p'-DDT) residues in catfish (Ictalurus punctatus) muscle tissue is presented. The 9 insecticides, plus dibutyl chlorendate internal standard, were fortified into catfish muscle tissue (0.5 g) and blended with 2 g C18 (octadecylsilyl derivatized silica reverse-phase material). The C18/muscle tissue matrix blend was fashioned into a column by adding the blend to a 10 mL syringe barrel containing 2 g activated Florisil. The insecticides were then eluted from the column with acetonitrile (8 mL), and a portion (2 microL) of the acetonitrile eluate was then directly analyzed by gas chromatography with electron capture detection. Unfortified blank controls were treated similarly. The resultant extracts contained pesticide analytes (31.25-500 ng/g) free of interfering compounds when analyzed. Correlation coefficients for the 9 extracted pesticide standard curves (linear regression analysis, n = 5) ranged from 0.9967 (+/- 0.0018) to 0.9999 (+/- 0.0001). Average percentage recoveries (82 +/- 4.8% to 97 +/- 3.6%, n = 25 for each insecticide), interassay (5.0 +/- 2.7% to 16.9 +/- 6.5%, n = 25 for each insecticide) and intraassay (1.8 to 4.7%, n = 5 for each insecticide) variabilities were indicative of an acceptable methodology for the analysis and screening of these residues in catfish muscle tissue.

摘要

本文介绍了一种多残留技术,用于提取鲶鱼(斑点叉尾鮰)肌肉组织中的9种杀虫剂(林丹、七氯、艾氏剂、七氯环氧化物、p,p'-滴滴伊、狄氏剂、异狄氏剂、p,p'-滴滴滴和p,p'-滴滴涕)残留并进行气相色谱筛查。将这9种杀虫剂以及氯菌酸二丁酯内标物添加到鲶鱼肌肉组织(0.5 g)中,与2 g C18(十八烷基硅烷衍生化硅胶反相材料)混合。通过将该C18/肌肉组织基质混合物添加到装有2 g活性弗罗里硅土的10 mL注射器筒中制成柱。然后用乙腈(8 mL)从柱中洗脱杀虫剂,取一部分(2 μL)乙腈洗脱液直接用带电子捕获检测的气相色谱进行分析。未添加杀虫剂的空白对照以类似方式处理。分析时,所得提取物含有无干扰化合物的农药分析物(31.25 - 500 ng/g)。9种提取农药标准曲线的相关系数(线性回归分析,n = 5)范围为0.9967(±0.0018)至0.9999(±0.0001)。平均回收率(每种杀虫剂n = 25,82 ± 4.8%至97 ± 3.6%)、批间变异(每种杀虫剂n = 25,5.0 ± 2.7%至16.9 ± 6.5%)和批内变异(每种杀虫剂n = 5,1.8至4.7%)表明该方法可用于分析和筛查鲶鱼肌肉组织中的这些残留。

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