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高效液相色谱-串联质谱内标法同时测定水产品中15种喹酮类药物残留量

ISSN号：1006-6144
期刊名称：《分析科学学报》
时间：0
分类：O657.63[理学—分析化学;理学—化学]
作者机构：[1]中国水产科学研究院黄海水产研究所,山东青岛266071
相关基金：国家863计划（No.2008AA100805）; 农业部行业专项（Nyhyzx07-046）; 基本科研业务费（2007-gy-02）

作者：王志杰[1], 冷凯良[1], 孙伟红[1], 宁劲松[1], 翟毓秀[1], 谭志军[1], 郭萌萌[1]

关键词：高效液相色谱-串联质谱, 内标法, 水产品, 喹诺酮类药物, 多残留同时测定, High performance liquid chromatography-tandem mass spectrometry, Internal standard method, Aquatic products, Quinolone, Multi-residue, Simultaneous determination

中文摘要：

建立了水产品中15种喹诺酮类药物（QNs）残留量的高效液相色谱-串联质谱（HPLC-MS/MS）测定方法。以氘代试剂为内标,样品经酸性乙腈萃取后,用正己烷脱脂,旋转蒸发浓缩,采用HPLC-MS/MS选择反应监测（SRM）正离子模式测定,内标法定量。可同时对水产品中的15种QNs进行定性和定量测定。15种QNs的检出限（S/N=3）为1.0μg/kg,定量限（S/N=10）为2.0μg/kg;在10.0～200.0ng/mL时峰强度与质量浓度的线性关系良好（r〉0.99）。方法的平均回收率范围为66%～121%。该法简便快捷,分析成本低,在一定程度上实现了药物残留的快速检测。

英文摘要：

A method for simultaneous determination of 15 QNs residues in aquatic products was developed by high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS）. Deuterium substituted reagents were added to the sample before extraction as internal standard. The sample was extracted with acidified acetonitril,cleaned-up with hexane,and concentrated with a rotary evaporator.The mass spectrometer was operated in positive ion mode using select reaction monitoring for qualitative and quantitative analysis of 15 QNs at the same time. The detection limits for 15 QNs were 1.0 μg/kg （S/N=3）,and the quantitation limits were 2.0 μg/kg （S/N=10）. The correlation coeficients of linear calibration curves were over 0.99 within the QNs concentration range 10.0~200.0 ng/mL. The average recoveries for 15 QNs were between 66% and 121%. The method features simple operation,low cost and fast analysis.