Simultaneous Determination of Five Carbamate Pesticides in Human Whole Blood by QuEChERS-Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry
摘 要
采用QuEChERS-超高效液相色谱-串联质谱法同时测定人全血中的灭多威、速灭威、残杀威、甲萘威、异丙威等5种氨基甲酸酯类农药。在1.00 mL全血样品中添加10 ng氘代灭多威作为内标物,加入2.00 mL乙腈和30 mg NaCl进行萃取,取上清液经复合吸附剂(150 mg无水MgSO4-25 mg N-丙基乙二胺-25 mg C18)净化后,采用ZORBAX Eclipse Plus C18色谱柱(2.1 mm×100 mm,1.8 μm)分离,以5 mmol·L-1乙酸铵溶液[含0.1%(体积分数)甲酸]和甲醇为流动相进行梯度洗脱,在电喷雾离子源正离子模式下电离,多反应监测模式下检测,以内标法定量。5种氨基甲酸酯类农药的质量浓度在一定范围内呈线性,检出限(3S/N)为0.10~0.50 μg·L-1,测定下限(10S/N)为0.50~0.75 μg·L-1。对空白全血样品进行加标回收试验,5种氨基甲酸酯类农药的回收率为87.5%~103%,测定值的相对标准偏差(n=6)为2.8%~7.9%。
Abstract
QuEChERS-ultra high performance liquid chromatography-tandem mass spectrometry was applied for the simultaneous determination of five carbamate pesticides (methomyl, metolcarb, propoxur, carbaryl and isoprocarb) in human whole blood. 10 ng of methomyl-D3 as an internal standard was added into 1.00 mL of whole blood sample, and the mixture was extracted with 2.00 mL of acetonitrile and 30 mg of NaCl. The supernatant was cleaned up with a composite adsorbent containing 150 mg of anhydrous MgSO4, 25 mg of N-(n-propyl)ethylenediamine and 25 mg of C18, then the analytes were separated on a ZORBAX Eclipse Plus C18 column (2.1 mm×100 mm, 1.8 μm) using a mixture of methanol and 5 mmol·L-1 ammonium acetate solution containing 0.1% (φ) formic acid as mobile phases for gradient elution. Electrospray positive ionization source was used. Analysis was practised under multiple reaction monitoring mode. Internal standard method was used for quantification. The linear relationships were found with the mass concentration of the five carbamate pesticides in definited ranges. The detection limits (3S/N) were in the range of 0.10-0.50 μg·L-1 and the lower limits of determination (10S/N) were in the range of 0.50-0.75 μg·L-1. Tests for recovery were made by standar addition method to blank sample, giving results between 87.5% and 103%, and RSDs (n=6) were in the range of 2.8%-7.9%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201812004
所属栏目 试验与研究
基金项目 公安部技术研究计划(2018JSYJC10);中央级公益性科研院所基本科研业务费项目(2018JB013)
收稿日期 2018/7/8
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备注万超超,硕士研究生,主要研究方向为毒物分析
引用该论文: WAN Chaochao,REN Xinxin,CHENG Fangbin,LÜ,Yufan,ZHENG Jiajia,HE Hongyuan. Simultaneous Determination of Five Carbamate Pesticides in Human Whole Blood by QuEChERS-Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(12): 1383~1388
万超超,任昕昕,程芳彬,吕昱帆,郑佳佳,何洪源. QuEChERS-超高效液相色谱-串联质谱法同时测定人全血中5种氨基甲酸酯类农药[J]. 理化检验-化学分册, 2018, 54(12): 1383~1388
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【3】蔡玉刚,苏晓虹,王运波.气相色谱法测定生物检材中的灭多威成份[J].广东公安科技, 2009,17(2):21-22.
【4】应剑波,谢伟宏,程建波,等.微波萃取-GPC净化-GC/MS法检验血中氨基甲酸酯和沙蚕毒素类农药[J].质谱学报, 2009,30(1):47-50.
【5】王媛,刘华良,朱宝立.高效液相色谱-串联质谱法测定血浆中的氨基甲酸酯类农药[J].中国卫生检验杂志, 2016,26(3):320-322.
【6】李鹏,柏泽新,夏侯秋锦,等.UPLC-MS/MS检测人血中18种有机磷及氨基甲酸酯类农药[J].中国法医学杂志, 2017,32(1):51-54.
【7】LIU S, PLEIL J D. Human blood and environmental media screening method for pesticides and polychlorinated biphenyl compounds using liquid extraction and gas chromatography-mass spectrometry analysis[J]. Journal of Chromatography B, 2002,769(1):155-167.
【8】李文海,朱鲁生.固相萃取GC/MS分析血中10种常见农药和杀鼠药[J].中国法医学杂志, 2009,24(4):269-271.
【9】ANASTASSIADES M, LEHOTAY S J, ŠTAJNBAHER D, et al. Fast and easy multiresidue method employing acetonitrile extraction/partitioning and "dispersive solid-phase extraction" for the determination of pesticide residues in produce[J]. Journal of AOAC International, 2003,86(2):412-431.
【10】GONZÁLEZ-CURBELO M Á, SOCAS-RODRÍGUEZ B, HERRERA-HERRERA A V, et al. Evolution and applications of the QuEChERS method[J]. TrAC-Trends in Analytical Chemistry, 2015,71:169-185.
【11】SCHMIDT M L, SNOW N H. Making the case for QuEChERS-gas chromatography of drugs[J]. TrAC-Trends in Analytical Chemistry, 2016,75:49-56.
【12】符靖雯,林玉婵,黄梅花,等.QuEChERS萃取结合GC-ECD测定甜玉米中多种有机氯及拟除虫菊酯类农药残留[J].理化检验-化学分册, 2017,53(9):1036-1041.
【13】WANG X C, SHU B, LI S, et al. QuEChERS followed by dispersive liquid-liquid microextraction based on solidification of floating organic droplet method for organochlorine pesticides analysis in fish[J]. Talanta, 2017,162:90-97.
【14】张晓强,张波,方萍,等.QuEChERS-超高效液相色谱-串联质谱法快速测定鱼肉中22种磺胺类药物残留[J].理化检验-化学分册, 2015,51(3):369-374.
【15】ARIAS J L O, SCHNEIDER A, BATISTA-ANDRADE J A, et al. Chitosan from shrimp shells:A renewable sorbent applied to the clean-up step of the QuEChERS method in order to determine multi-residues of veterinary drugs in different types of milk[J]. Food Chemistry, 2018,240:1243-1253.
【16】MYRESIOTIS C K, TESTEMPASIS S, VRYZAS Z, et al. Determination of mycotoxins in pomegranate fruits and juices using a QuEChERS-based method[J]. Food Chemistry, 2015,182:81-88.
【17】陈建彪,董丽娜,刘娇,等.QuEChERS在食品中真菌毒素检测的研究进展[J].食品科学, 2014,35(11):286-291.
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