气相色谱法测定土豆中8种有机氯农药残留.docVIP

气相色谱法测定土豆中8种有机氯农药残留 　　摘要 研究了土豆中的8种有机氯农药（包括α-666、β-666、γ-666、δ-666、o，p’-DDE、p，p’-DDE、o，p’-DDD、o，p’-DDT）残留量的气相色谱测定方法。采用乙腈提取，弗罗里矽柱柱净化，HP-5柱色谱分离，ECD检测器检测，基质匹配外标法定量。8种有机氯农药在13 min内获得良好的分离，8种有机氯农药在0.05～1.00 mg/L浓度范围内均有良好的线性关系，相关系数不低于0.999 57，加标回收率为83.1%～106.5%，相对标准偏差在（n=7）2.8%～9.7%之间。该法快速灵敏，且易操作。 　　关键词 气相色谱法；土豆；有机氯农药；残留量 　　中图分类号 X839.2 文献标识码 A 文章编号 1007-5739（2016）04-0120-01 　　Determination of 8 Organochlorine Pesticides Residue in Potato by Using Gas Chromatography 　　WU Xing-xiang 1 YANG Juan 1 LI Xiao-peng 2 * CHEN Nan 2 MA Shi-zhu 2 FENG Min-ling 3 　　（1 Sanshui District Agricultural Products Quality and Security Inspection Center of Foshan City in Guangdong Province，Foshan Guangdong 528100； 　　2 Sanxiang Town Inspection and Testing Station of Agricultural Products in Zhongshan City； 3 Zhongshan Quality Supervision Inspection Institute of Agricultural Products） 　　Abstract A method for determination of 8 organochlorine pesticides residue（including α-666、β-666、γ-666、δ-666、o，p’-DDE、p，p’-DDE、o，p’-DDD、o，p’-DDT）in potato by gas chromatography was investigated.The eight pesticides could be well separated within 13 min in a HP-5 column after being extracted with acetonitrile and cleaned up by solid-phase florisil column.The pesticides were detected with ECD detector. A matrix matched external standard was used for quantitative analysis. The calibration curves were in good linearity between the peak area and the concentration of 0.05～1.00 mg/L for 8 organochlorine pesticides with correlation coefficients not less than 0.999 57.The spiked recoveries ranged from 83.1% to 106.5% with RSD′s（n=7）in the range of 2.8%～9.7%. The method was quick，sensitive and easy in operation. 　　Key words gas chromatography；potato；organochlorine pesticide；residue 　　土豆，又称地蛋、马铃薯、洋山芋等，属茄科多年生草本植物，块茎可供食用，是全球第四大重要的粮食作物，仅次于小麦、稻谷和玉米。中国是世界上土豆总产量最多的国家。 　　由于土豆生长在地下土壤中，残留于土壤的农药会被土豆吸收，同时土豆病虫害的防治在一定程度上也依赖于农药，其残留给大气和土壤带来了严重的影响[1-2]。因此，建立一种快速、准确测定土豆中有机氯多农药残留检测方法具有重要意义。 　　1 材料与方法 　　1.1 仪器与试剂 　　Agilent