黄芪及其种植土壤中毒杀芬残留量的测定方法  

Determination of toxaphene in astragalus mongholicus and soil

作　　者：徐宜宏 黄莹滢[2] 郭松 毕孝瑞 张敏 付海滨[2] 陈富于[1] 陈丽静[1] XU Yihong;HUANG Yingying;GUO Song;BI Xiaorui;ZHANG Min;FU Haibin;CHEN Fuyu;CHEN Lijing(College of Engineering,Shenyang Agricultural University,Shenyang 1108GG,China;Shenyang Entry Exit Inspection and Quarantine Bureau,Shenyang 110016,China)

机构地区：[1]沈阳农业大学工程学院,沈阳110866 [2]沈阳出入境检验检疫局,沈阳110016

出　　处：《沈阳师范大学学报（自然科学版）》2018年第2期185-188,共4页Journal of Shenyang Normal University:Natural Science Edition

基　　金：国家质检总局科技计划项目(2014IK153);沈阳市科技计划项目(17-159-8-00)

摘　　要：建立了中国传统经典中药材黄芪及其种植土壤中毒杀芬残留量的气相色谱-电子捕获检测器检测方法。粉碎后的黄芪和土壤样品采用正己烷提取毒杀芬后,提取液经PSA(N-丙基乙二胺)和石墨化炭黑固相萃取填料净化,气相色谱-电子捕获检测器测定其毒杀芬含量,外标法定量。方法定量限(信噪比为10∶1)为0.01mg/kg,在0.1~2.0μg/mL的质量浓度范围内,相关系数为0.996,在黄芪和土壤2种样品基质中,0.01,0.02,0.10mg/kg 3个添加水平下,分别平行测定6次,回收率为81%~98%,相对标准偏差(RSD)为2.3%~5.3%,均符合农药残留检测要求。该方法提取效果好,检测灵敏度高,适用于黄芪及其种植土壤中毒杀芬的快速检测。A method was developed for the determination of toxaphene residues in Chinese traditional medicine astragalus mongholicus and soil by capillary gas chromatographic-electron capture detector.The pesticide in the pulverized samples was extracted using n-hexane and purified by PSA and Carb,finally detected by GC-electron capture detector,external standard method for quantitative.The quantization limit（S/N=10∶1）found was 0.01 mg/kg.In the linear range of 0.1-2.0μg/mL,the correlation coefficient was 0.996.The performance was demonstrated by the analysis of astragalus mongholicus and soil samples spiked with toxaphene congeners at three levels of 0.01、0.02、0.10 mg/kg（n=6）,the corresponding recoveries were 81% -98%,the relative standard deviations（RSD）were 2.3%-5.3%,all conforms to the requirement of pesticide residue detection.This method is sensitive and efficient in the aspect of extraction,and suitable for rapid detection of toxaphene residues in astragalus mongholicus and soil.

关 键 词：黄芪 土壤 毒杀芬 气相色谱 农药残留 

分 类 号：O6[理学—化学]