气相色谱-质谱法测定生活饮用水中23种有机磷农药的含量
GC-MS Determination of 23 OPPs in Drinking Water
摘 要
将搅拌棒置于20 mL顶空瓶中，向顶空瓶中加入水样18 mL和甲醇2 mL，盖紧盖子，以转速800 r·min-1于20℃下搅拌溶液20 min。取出搅拌棒，将其放入热脱附玻璃管中。解吸液以DB-5MS色谱柱为固定相进行气相色谱分离。质谱分析中采用选择离子监测模式。23种有机磷农药的质量浓度在0.05~5.00 mg·L-1范围内与其峰面积呈线性关系，检出限（3S/N）为0.3~25 μg·L-1。按标准加入法在3个浓度水平上进行回收试验，回收率在70.9%~97.1%之间，测定值的相对标准偏差（n=6）均小于5.5%。
搅拌棒吸附萃取
热脱附
有机磷农药
生活饮用水
GC-MS
stir bar sorptive extraction
thermal desorption
OPPs
drinking water
Abstract
The stir bar was placed in 20 mL of a headspace bottle, and 18 mL of water sample and 2 mL of methanol were added into the headspace bottle. After closed the lip, the solution was stirred for 20 min at 20℃ with the speed of 800 r·min-1. The stir bar was taken out and placed into the thermal desorption glass tube. Desorption solution was separated by GC using DB-5MS chromatographic column as stationary phase. SIM was adopted in MS analysis. Linear relationships between values of peak area and mass concentration of 23 OPPs were found in the range of 0.05-5.00 mg·L-1, with detection limits (3S/N) in the range of 0.3-25 μg·L-1. Test for recovery was made by standard addition at 3 concentration levels, giving results in the range of 70.9%-97.1%, with RSDs (n=6) all less than 5.5%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201710013
所属栏目 工作简报
基金项目 淮安市科技局科技计划项目（社会发展）（HAS2015030）；淮安市预防医学科研课题项目（hayf201513）
收稿日期 2016/12/27
修改稿日期
网络出版日期
作者单位点击查看
备注王芹(1982-),女,江苏淮安人,主管技师,本科,主要从事理化检验工作
引用该论文: WANG Qin,HANG Xueyu,SONG Xin,WANG Lu,FENG Xiaoqing,XU Rui,LI Lei. GC-MS Determination of 23 OPPs in Drinking Water[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2017, 53(10): 1182～1187
王芹,杭学宇,宋鑫,王露,冯晓青,徐瑞,李磊. 气相色谱-质谱法测定生活饮用水中23种有机磷农药的含量[J]. 理化检验－化学分册, 2017, 53(10): 1182～1187
共有人对该论文发表了看法，其中：
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】俞发荣,李登楼.有机磷农药对人类健康的影响及农药残留检测方法研究进展[J].生态科学, 2015,34(3):197-203.
【2】雷昌文,曹莹,周腾耀,等.太湖水体中5种有机磷农药混合物生态风险评价[J].生态毒理学报, 2013,8(6):937-944.
【3】郭强,田慧,毛潇萱,等.珠江河口水域有机磷农药水生生态系统风险评价[J].环境科学, 2014,35(3):1029-1034.
【4】李晓亚,张永涛,张莉,等.固相萃取-气相色谱法测定水中有机磷农药[J].理化检验-化学分册, 2013,49(7):820-823.
【5】胡红美,郭远明,金衍健,等.固相膜萃取-气相色谱法测定养殖用水中痕量有机磷农药[J].理化检验-化学分册, 2015,51(6):770-774.
【6】FARAJZADEH M A, ASGHARI A, FERIDUNI B. An efficient, rapid and microwave-accelerated dispersive liquid-liquid microextraction method for extraction and pre-concentration of some organophosphorus pesticide residues from aqueous samples[J]. Journal of Food Composition & Analysis, 2016,48:73-80.
【7】黄倩,何蔓,陈贝贝,等.磁固相萃取-气相色谱-火焰光度检测联用测定果汁中的有机磷农药[J].色谱, 2014,32(10):1131-1137.
【8】钱飞中,陈钟佺,冯加永,等.填充吸附微萃取-气相色谱法检测水中有机磷农药[J].分析试验室, 2015(6):630-634.
【9】黄惠玲,王玉健,黄海民,等.气相色谱法测定水果和蔬菜中5种有机含磷农药的残留量[J].理化检验-化学分册, 2012,48(7):836-838.
【10】徐玉娥,魏远隆,左海根,等.低温富集液液萃取-气相色谱-串联质谱法测定水样中15种农药残留[J].理化检验-化学分册, 2015,51(1):1-5.
【11】ZAMBONIN C G, QUINTO M, VIETRO N D, et al. Solid-phase microextraction-gas chromatography mass spectrometry:A fast and simple screening method for the assessment of organophosphorus pesticides residues in wine and fruit juices[J]. Food Chemistry, 2004,86(2):269-274.
【12】姚铭栋.饮用水中多种有机磷农药残留的气相色谱-三重四极杆质谱测定法[J].职业与健康, 2014,30(18):2578-2579.
【13】魏天龙.高效液相色谱法同时测定生活饮用水中七种有机磷农药残留研究[D].兰州:西北师范大学, 2013.
【14】张磊,王红斌,李彬,等.水环境中15种农药残留的固相萃取-高效液相色谱分析方法[J].环境化学, 2013,32(8):1584-1585.
【15】孙志伟.环境水体农药残留量的高效液相色谱法测定[J].科技创新导报, 2015,12(21):130-131.
【16】付慧,张海婧,胡小键,等.水中呋喃丹及5种有机磷农药的超高效液相色谱串联质谱测定法[J].环境与健康杂志, 2015,32(3):243-246.
【17】刘莹雯,丁时超,杜文,等.高效液相色谱-串联质谱法测定烟草中有机磷农药的残留量[J].色谱, 2006,24(2):174-176.
【18】DIETZ C, SANZ J, CÁMARA C. Recent developments in solid-phase microextraction coatings and related techniques[J]. Journal of Chromatography A, 2006,1103(2):183-192.
【19】陈宗保,刘林海,叶青.饮用水中12种有机磷及氨基甲酸酯类农药残留量的气相色谱-质谱测定法[J].环境与健康杂志, 2009,26(2):156-158.
【2】雷昌文,曹莹,周腾耀,等.太湖水体中5种有机磷农药混合物生态风险评价[J].生态毒理学报, 2013,8(6):937-944.
【3】郭强,田慧,毛潇萱,等.珠江河口水域有机磷农药水生生态系统风险评价[J].环境科学, 2014,35(3):1029-1034.
【4】李晓亚,张永涛,张莉,等.固相萃取-气相色谱法测定水中有机磷农药[J].理化检验-化学分册, 2013,49(7):820-823.
【5】胡红美,郭远明,金衍健,等.固相膜萃取-气相色谱法测定养殖用水中痕量有机磷农药[J].理化检验-化学分册, 2015,51(6):770-774.
【6】FARAJZADEH M A, ASGHARI A, FERIDUNI B. An efficient, rapid and microwave-accelerated dispersive liquid-liquid microextraction method for extraction and pre-concentration of some organophosphorus pesticide residues from aqueous samples[J]. Journal of Food Composition & Analysis, 2016,48:73-80.
【7】黄倩,何蔓,陈贝贝,等.磁固相萃取-气相色谱-火焰光度检测联用测定果汁中的有机磷农药[J].色谱, 2014,32(10):1131-1137.
【8】钱飞中,陈钟佺,冯加永,等.填充吸附微萃取-气相色谱法检测水中有机磷农药[J].分析试验室, 2015(6):630-634.
【9】黄惠玲,王玉健,黄海民,等.气相色谱法测定水果和蔬菜中5种有机含磷农药的残留量[J].理化检验-化学分册, 2012,48(7):836-838.
【10】徐玉娥,魏远隆,左海根,等.低温富集液液萃取-气相色谱-串联质谱法测定水样中15种农药残留[J].理化检验-化学分册, 2015,51(1):1-5.
【11】ZAMBONIN C G, QUINTO M, VIETRO N D, et al. Solid-phase microextraction-gas chromatography mass spectrometry:A fast and simple screening method for the assessment of organophosphorus pesticides residues in wine and fruit juices[J]. Food Chemistry, 2004,86(2):269-274.
【12】姚铭栋.饮用水中多种有机磷农药残留的气相色谱-三重四极杆质谱测定法[J].职业与健康, 2014,30(18):2578-2579.
【13】魏天龙.高效液相色谱法同时测定生活饮用水中七种有机磷农药残留研究[D].兰州:西北师范大学, 2013.
【14】张磊,王红斌,李彬,等.水环境中15种农药残留的固相萃取-高效液相色谱分析方法[J].环境化学, 2013,32(8):1584-1585.
【15】孙志伟.环境水体农药残留量的高效液相色谱法测定[J].科技创新导报, 2015,12(21):130-131.
【16】付慧,张海婧,胡小键,等.水中呋喃丹及5种有机磷农药的超高效液相色谱串联质谱测定法[J].环境与健康杂志, 2015,32(3):243-246.
【17】刘莹雯,丁时超,杜文,等.高效液相色谱-串联质谱法测定烟草中有机磷农药的残留量[J].色谱, 2006,24(2):174-176.
【18】DIETZ C, SANZ J, CÁMARA C. Recent developments in solid-phase microextraction coatings and related techniques[J]. Journal of Chromatography A, 2006,1103(2):183-192.
【19】陈宗保,刘林海,叶青.饮用水中12种有机磷及氨基甲酸酯类农药残留量的气相色谱-质谱测定法[J].环境与健康杂志, 2009,26(2):156-158.
相关信息
