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    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

    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%.

       

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