固相萃取-气相色谱法同时测定花生中18种有机氯农药残留

利用气相色谱(GC)建立了花生中18种有机氯农药同时测定的方法。花生中有机氯农药残留通过乙腈提取,减压浓缩后过弗罗里固相萃取柱净化,采用正己烷-丙酮(体积比为9∶1)溶液淋洗,淋洗液氮吹近干后以正己烷定容,应用微池电子捕获检测器(μECD)检测。氟氯氰菊酯和溴氰菊酯的检出限分别为50和100g/kg,其余16种有机氯农药检出限均为10μg/kg。在花生样品中添加检测限水平有机氯混标溶液,加标回收率为71.28%～116.58%,测定结果的相对标准偏差为4.08%～18.16%(n=4或5)。

SIMULTANEOUS DETERMINATION OF 18 KINDS OF ORGANOCHLORINE PESTICIDES RESIDUES IN PEANUT BY SOLID-PHASE EXTRACTION AND GAS CHROMATOGRAPHY

A method was developed for the simultaneous determination of 18 kinds of organochlorine pesticide residues in peanut with solid - phase extraction and gas chromatograph. Residues were extracted from peanut sample with acetonitrile, purified through florisil SPE column and washed with hexane - acetone （ volume ratio was 9：1 ）. Elution liquid was diluted with hexane to volume after nitrogen blowing just to dryness, then the residues in it was analyzed by gas chromatograph with mierocell electron capture detector. The detection limits were 50 and 100 μg/kg for cyfluthrin and dehamethrin respectively, and the remaining 16 kinds of organo- chlorine pesticides residue detection limits were 10μg/kg. The adding recoveries ranged from 71.28% to 116.58% , and the relative standard deviations of repeatability detection results were 4.08% - 18.16% （n = 4 or 5 ）.