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[固相萃取-毛细管气相色谱法测定九种中药材中有机氯农药残留量]

[Determination of organochlorine pesticide residues in nine herbs by solid-phase extraction and capillary gas chromatography].

作者信息

Yan Zheng, Feng Di, Li Shenjie, Zhao Yakui, Yang Hui

机构信息

College of Chemistry and Environmental Science, Hebei University, Baoding 071002, China.

出版信息

Se Pu. 2005 May;23(3):308-11.

Abstract

The solid-phase extraction and capillary gas chromatography was introduced for determining 13 organochlorine pesticide residues including alpha-benzene hexachloride (BHC), betaBHC, gamma-BHC, delta-BHC, p,p'-dichloro-diphenyl-dichloroethylene (pp'-DDE), p,p'-dichloro-di-phenyl-dichloroethane (pp'-DDD), o,p'-dichloro-diphenyl-trichloroethane (op'-DDT), pp'-DDT, heptachlor (HEPT), aldrin, heptachlor epoxide (HCE), dieldrin and endrin in Scutellaria baicalensis, Salvia miltiorrhiza, Belamcanda chinensis, Paeoniae lactiflora, Angelica dahurica, Arisaema erubescens, Fructus arctii, Anemarrhena asphodeloides and Platycodon grandiflorum. The organochlorine pesticides were extracted from herbs with mixed solvents of acetone and n-hexane by ultrasonic and cleaned up by Florisil solid-phase extraction column. Then, the extract was separated by capillary column (30 m x 0.25 mm i.d. x 0.25 microm) and detected by electrochemical detector. The carrier gas was N2 (99.999%) with the flow rate of 1.4 mL/min. The split ratio was 1:2.2. The injector temperature was 220 degrees C and the detector temperature was 330 degrees C. The column temperature was increased by the rate of 20 degrees C/min from 100 degrees C to 190 degrees C (hold for 1. 0 min), then to 235 degrees C by the rate of 4 degrees C/min and hold for 7 min at 235 degrees C. The good linearities were obtained for 13 organochlorine pesticides. The detection limits were between 0.064-0.61 microg/L. The average recoveries were between 87.3%-102.3% and relative standard deviations of 1.3%-6.8%. The method is effective, fast and accurate.

摘要

采用固相萃取和毛细管气相色谱法测定黄芩、丹参、射干、白芍、白芷、天南星、牛蒡子、知母和桔梗中13种有机氯农药残留,包括α-六六六(BHC)、β-六六六、γ-六六六、δ-六六六、p,p'-二氯二苯二氯乙烯(pp'-DDE)、p,p'-二氯二苯二氯乙烷(pp'-DDD)、o,p'-二氯二苯三氯乙烷(op'-DDT)、pp'-DDT、七氯(HEPT)、艾氏剂、环氧七氯(HCE)、狄氏剂和异狄氏剂。有机氯农药用丙酮和正己烷混合溶剂超声提取,经弗罗里硅土固相萃取柱净化。然后,提取物用毛细管柱(30 m×0.25 mm内径×0.25μm)分离,电化学检测器检测。载气为N2(99.999%),流速为1.4 mL/min。分流比为1:2.2。进样口温度为2​​20℃,检测器温度为330℃。柱温以20℃/min的速率从100℃升至190℃(保持1.0 min),然后以4℃/min的速率升至235℃,并在235℃保持7 min。13种有机氯农药具有良好的线性关系。检测限在0.0​​64 - 0.61μg/L之间。平均回收率在87.3% - 102.3%之间,相对标准偏差为1.3% - 6.8%。该方法有效、快速、准确。

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