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液相色谱-串联质谱法测定肉品中氯噻啉药物残留 预览

Determination of Imidaclothiz Residues in Meat by Liquid Chromatography-Tandem Mass Spectrometry
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摘要 采用液相色谱-串联质谱(liquid chromatography-tandem mass spectrometry,LC-MS/MS)法测定肉品中氯噻啉药物残留。肉样经过酸化乙腈提取后,采用N-丙基乙二胺和C_(18)吸附剂净化,然后在BEH-C18柱(2.1 mm×50 mm,1.7 μm)上用乙腈和体积分数为0.1%的甲酸水溶液为流动相进行梯度洗脱,流速0.30 mL/min。样品经电喷雾离子源正离子模式电离后,在多反应监测模式下定性及定量。结果表明:该方法在10-400 ng/mL范围内线性关系良好,方法检出限为5.0 μg/kg,回收率为91.41%-93.51%,相对标准偏差在2.4%-3.2%之间。该方法结合了QuEChERS(quick,easy,cheap,effective,rugged,safty)和LC-MS/MS的优点,操作简便、分析速度快、灵敏度高、重现性好,可以用于肉品中氯噻啉残留的检测。 This paper presents a method for the determination of imidaclothiz residue in meat by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Samples were extracted with acidic acetonitrile, and the extract was then cleaned up with primary secondary amine (PSA) and C18 sorbent. The separation was performed on a BEH-C18 column (2.1 mm × 50 mm, 1.7 μm) using gradient elution with acetonitrile and 0.1% formic acid in water as mobile phase at a flow rate of 0.30 mL/min. The analyte was detected with an electrospray ionization source in the positive ion mode (ESI+) using multiple reaction monitoring (MRM). The results showed that the developed method exhibited good linearity over the concentration range of 10-400 ng/mL. The limit of detection was 5.0 μg/kg, and the recovery was 91.41%-93.51% with relative standard deviation between 2.4% and 3.2%. This method, combining the advantages of both QuEChERS (quick, easy, cheap, effective, rugged, safty) and LC-MS/MS such as simplicity, rapidity, high sensitivity, and good reproducibility, can be used for the determination of imidaclothiz residue in meat.
作者 周大卫 ZHOU Dawei (Beijing Supervision and Testing Center One Station for Foods and Alcoholic Products, Beijing 100075, China)
出处 《肉类研究》 北大核心 2018年第3期51-55,共5页 Meat Research
关键词 氯噻啉 残留分析 液相色谱-串联质谱 QUECHERS 肉品 imidaclothiz residues analysis liquid chromatography-tandem mass spectrometry QuEChERS meat
作者简介 周大卫(1984-),男,工程师,本科,研究方向为食品检测。E—mail:david6622@foxmail.com.
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