多残留基质固相分散(MSPD)提取和气相色谱法筛选鲶鱼肌肉组织中9种氯农药。

A R Long, M D Crouch, S A Barker
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引用次数: 0

摘要

建立了林丹、七氯、艾氏剂、环氧七氯、p,p′-DDE、狄氏剂、endrin、p,p′-TDE、p,p′-滴滴涕等9种杀虫剂在鲶鱼肌肉组织中的多残留提取和气相色谱筛选技术。将9种杀虫剂加氯酸二丁酯内标剂掺入鲶鱼肌肉组织(0.5 g)中,与C18(十八烷基硅基衍生二氧化硅反相材料)2 g混合。将C18/肌肉组织基质混合物加入含有2g活化Florisil的10ml注射器桶中,制成柱状。用乙腈(8 mL)洗脱柱上的杀虫剂,用电子捕获检测气相色谱法直接分析一部分(2微l)乙腈洗脱液。未强化的空白对照同样处理。所得提取物含有农药分析物(31.25-500 ng/g),分析时无干扰化合物。9条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)~ 0.9999(+/- 0.0001)。平均回收率(82 +/- 4.8% ~ 97 +/- 3.6%,每种杀虫剂的n = 25)、测定间(5.0 +/- 2.7% ~ 16.9 +/- 6.5%,每种杀虫剂的n = 25)和测定内(1.8 ~ 4.7%,每种杀虫剂的n = 5)的变异率表明,这是一种可接受的方法,用于分析和筛选鲶鱼肌肉组织中这些残留物。
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Multiresidue matrix solid phase dispersion (MSPD) extraction and gas chromatographic screening of nine chlorinated pesticides in catfish (Ictalurus punctatus) muscle tissue.

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.

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