搅拌棒吸附萃取-液相色谱-串联质谱法测定微山湖水中的有机磷农药残留
Determination of Organophosphorus Pesticide Residues in Weishan Lake Water by LC-MS/MS Combined with Stir Bar Sorptive Extraction
摘 要
采用搅拌棒吸附萃取结合液相色谱-串联质谱法测定微山湖水中的马拉硫磷、三唑磷、喹硫磷、伏杀硫磷等4种有机磷农药残留。对影响有机磷农药残留吸附萃取效率的萃取涂层、样品溶液的酸度、振荡速率、萃取时间、溶液的离子强度、解吸液、解吸时间和解吸模式等因素进行了优化,确定了最佳吸附萃取条件。样品经搅拌棒萃取、解吸后,采用ZORBAX Eclipse Plus C18色谱柱分离,在多反应监测模式下检测,外标法定量。4种有机磷农药的质量浓度在一定范围内与峰面积呈线性关系,检出限(3S/N)在0.16~0.73 μg·kg-1之间。加标回收率在72.3%~107%之间,测定值的相对标准偏差(n=6)在7.8%~11%之间。
搅拌棒吸附萃取
有机磷
残留
微山湖水
LC-MS/MS
Stir bar sorptive extraction
Organophosphorus
Residue
Weishan Lake water
Abstract
LC-MS/MS coupled with stir bar sorptive extraction (SBSE) was applied to the determination of 4 organophosphorus pesticides residues, including malathion, triazophos, quinalphos and phosalone, in Weishan Lake water. The optimum extraction condition was achieved by optimizing the factors of SBSE efficiency, such as extraction coating, acidity of the sample solution, stirring speed, extraction time, ionic strength of the solution, desorption solution, desorption time and desorption mode. After the sample was extracted by SBSE and desorption, the analytes were separated on a ZORBAX Eclipse Plus C18 chromatographic column. The MS analysis was carried out in the multi reaction monitoring mode and external standard method was used for quantification. Linear relationships were found between the peak areas and the mass concentrations of the 4 organophosphorus pesticides in definited ranges with the detection limits (3S/N) in the range of 0.16-0.73 μg·kg-1. Recovery rates obtained by standard addition method were in the range of 72.3%-107% and RSDs (n=6) were in the range of 7.8%-11%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201607005
所属栏目 工作简报
基金项目 山东检验检疫局科研项目(SK201232;SK201426)
收稿日期 2015/6/24
修改稿日期
网络出版日期
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备注倪永付(1983-),男,山东微山人,硕士,研究方向为 化学分析。
引用该论文: NI Yong-fu,YAN Qiu-cheng,ZHU Li-ping. Determination of Organophosphorus Pesticide Residues in Weishan Lake Water by LC-MS/MS Combined with Stir Bar Sorptive Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2016, 52(7): 766～769
倪永付,闫秋成,朱莉萍. 搅拌棒吸附萃取-液相色谱-串联质谱法测定微山湖水中的有机磷农药残留[J]. 理化检验－化学分册, 2016, 52(7): 766～769
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【3】曹赵云,牟仁祥,吴俐,等.程序升温大体积进样和解卷积气相色谱-质谱法测定蔬菜水果中32种农药残留量［J］.色谱, 2014,32(12):1390-1399．
【4】杜晓婷,周敏,张剑,等.蔬菜中甲胺磷等5种有机磷农药残留量的分散液-液微萃取气质联用技术检测［J］.分析测试学报, 2010,29(7):751-754．
【5】楼小华,高川川,朱文静,等.GC-MS-MS法同时测定烟草中113种有机磷、有机氯及拟除虫菊酯类农药残留［J］.中国烟草科学, 2012,33(5):83-89．
【6】姜欣.4种常用有机磷农药反相高效液相色谱分析［J］.农药, 2009,48(4):272-273．
【7】刘永,唐英斐,宋金凤,等.固相萃取-液相色谱-串联质谱法测定蔬菜中4种有机磷农药及其代谢产物［J］.色谱, 2014,32(2):139-144．
【8】王玉健,黄惠玲,董存柱,等.超高效液相色谱-串联质谱法同时测定水产品中9种有机磷农药残留量［J］.理化检验-化学分册, 2013,49(4):398-401．
【9】王玉健,黄惠玲,林正锋,等.超高效液相色谱-串联质谱法同时测定水果中吡菌磷等9种有机磷农药残留量［J］.分析试验室, 2011,30(10):88-91．
【10】邹泊羽,熊越.搅拌棒吸附萃取技术及其在食品分析中的应用［J］.粮油食品科技, 2011(3):58-61．
【11】HUANG X J, QIU N N, YUAN D X, et al. Simple and sensitive monitoring of sufonamide veterinary residues in milk by stir bar sorptive extraction based on monolithic material and high performance liquid chromatography analysis［J］. Journal of Chromatography A, 2009,1216(46):8240-8245．
【12】许志刚,胡玉玲,李攻科.搅拌棒吸附萃取技术的研究进展［J］.分析化学, 2011(11):1766-1773．
【13】BENED J L, CHISVERT A, GIOKAS D L, et al. Development of stir bar sorptive-dispersive micro-extraction mediated by magnetic nanoparticles and its analytical application to the determination of hydrophobic organic compounds in aqueous media［J］. Journal of Chromatography A, 2014,1362:25-33．
【14】ASSOUMANI A, MARGOUM C, CHATAING S, et al. Use of passive stir bar sorptive extraction as a simple integrative sampling technique of pesticides in freshwaters: determination of sampling rates and lag-phases［J］. Journal of Chromatography A, 2014,1333:1-8．
【15】倪永付,闫秋成,朱莉萍.一种搅拌棒吸附萃取及解析装置:201320611704.3［P］. 2014-03-12．
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