Simultaneous Determination of 30 Pesticide Residues in Soil by GC-MS
摘 要
采用气相色谱-质谱法同时测定土壤中30种农药残留.样品经过丙酮-正己烷(1+1)混合溶液均质提取,再用正己烷进行萃取,弗罗里硅土柱净化后,采用HP-5MS色谱柱分离,选用电子轰击离子源和选择离子监测模式进行质谱分析,外标法定量.30种农药的线性范围为0.1~1.0 mg·L-1,检出限(3S/N)为3.8~9.6 μg·kg-1.加标回收率在75.8%~103%之间,测定值的相对标准偏差(n=6)在5.6%~9.7%之间.
Abstract
A GC-MS method was developed for the determination of 30 pesticide residues in soil.The sample was extracted with acetonen-hexane (1+1) and hexane in succession.Then the extract was cleaned up on a florisil cartridge and separated on a HP-5MS column.EI-SIM was adopted in MS and external standard was used for quantification.The linearity range of 30 pesticide residues was 0.1-1.0 mg·L-1 with detection limits (3S/N) in the range of 3.8-9.6 μg·kg-1.The recovery rates measured by standard addition method were in the range of 75.8%-103% and RSD (n=6) were in the range of 5.6%-9.7%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201507008
所属栏目 工作简报
基金项目 国家质检总局科研项目(2012IK176);山东检验检疫局科研项目(SK201353)
收稿日期 2014/7/23
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备注高玉生(1982-),男,山东烟台人,助理工程师,主要研究方向为食品中药物残留检测.
引用该论文: GAO Yu-sheng,LI Xiao-yu,YU Jie,LI Shu-juan,LI Miao,DUAN Xiao-hui. Simultaneous Determination of 30 Pesticide Residues in Soil by GC-MS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(7): 925~929
高玉生,李晓玉,于杰,李淑娟,李淼,段效辉. 气相色谱-质谱法同时测定土壤中30种农药残留[J]. 理化检验-化学分册, 2015, 51(7): 925~929
被引情况:
【1】吴春英,白鹭,谷风,陆文龙, "固相萃取-超高效液相色谱-串联质谱法同时测定地表水中的18种酰胺类除草剂",理化检验-化学分册 52, 602-606(2016)
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参考文献
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【2】闫蕊,邵明媛,鞠福龙,等.加速溶剂萃取-高效液相色谱串联质谱法测定土壤中农药残留[J].分析化学,2013,41(2):315-316.
【3】陈啓荣,郎爽,魏岩,等.加速溶剂萃取-凝胶色谱净化-气质联用测定土壤中15种有机氯农药残留的方法研究[J].分析测试学报,2010,29(5):473-477.
【4】谢湘云,沈爱斯,叶江雷,等.固相萃取小柱净化-气相色谱法测定土壤和沉淀物中有机氯和拟除虫菊酯农药残留[J].环境化学,2006,25(3):347-340.
【5】尤继明,李红梅,范明红,等.凝胶色谱净化-气相色谱法测定土壤中六六六和滴滴涕残留[J].安徽农学通报,2012,18(11):34-36.
【6】陈必群,林玉清,楼建华.气相色谱法同时测定土壤中10种有机氯农药残留量[J].理化检验-化学分册,2006,42(9):729-731.
【7】董冀川,杨琼.气相色谱法同时分析土壤中15种有机氯农药残留[J].中国环境监测,2009,25(4):7-10.
【8】万益群,陈宗保.土壤中多种有机磷及氨基甲酸酯类农药残留量的气相色谱-质谱法测定[J].分析化学学报,2006,22(5):551-514.
【9】李俊,肖雅雯,王震,等.加速溶剂萃取-气相色谱/质谱法同时测定土壤中拟除虫菊酯类等18种农药残留[J].岩矿测试,2011,30(5):590-595.
【10】GONCALVES C,ALPENDURADA M F.Assessment of pesticide contamination in soil sample from an intensive horticulture area using jultrasonic extraction and gas chromatography-mass spectrometry[J].Talanta,2005,65(5):1179-1189.
【11】黄文军,高丽荣,弓爱君,等.同位素稀释高分辨气相色谱-高分辨质谱法测定土壤中痕量有机氯农药残留[J].色谱,2010,28(5):460-464.
【12】贾丽娟,邓芸芸.气相色谱-串联质谱法测定土壤中的有机氯农药[J].色谱,2008,26 (6):697-703.
【13】张新忠,罗逢健,陈宗懋,等.超高效液相色谱串联质谱法测定茶叶、茶汤和土壤中氟环唑、茚虫威和苯醚甲环唑残留[J].分析化学,2013,41(2):215-222.
【14】沈菁,刘军,陈平,等.液相色谱-质谱法测定土壤和甘蓝中的虫酰肼残留[J].湖北农业科学,2009,2(48):442-444.
【15】BLASCO C,VAZQUEZ-ROIG P,ONGHENA ,et al.Analysis of insecticides in honey by liquid chromatography-ion trap-mass spectrometry:Comparison of different extraction procedures[J].Journal of Chromatography A,2011,1218(30):4892-4901.
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