高效液相色谱-四极杆-飞行时间质谱法筛查中华鳖中42种兽药残留
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李诗言(1987-),男,硕士,助理工程师,研究方向为水产品质量与安全,jimmyuu1987@163.com

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2013年浙江省农业标准化研究项目


Rapid screening and confirmation of 42 veterinary drugs in Chinese softshell turtle by liquid chromatography/quadrupole time-of-flight mass spectrometry
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    摘要:

     建立了中华鳖中42种兽药残留的液相色谱-四极杆/飞行时间质谱(LC-Q-TOF/MS)快速筛查方法。采用乙腈/水(6∶4, V/V)提取样品,经HLB柱吸附净化后上机。质谱正离子扫描模式下,10 min内42种药物得以色谱分离,所有药物在线性范围内线性良好,定量限范围为5~50 μg/kg,3个添加水平(n=6)下的平均回收率为56.8%~103.8%,相对标准偏差(RSD)为1.26%~10.01%。本方法采用精确质量数据库和二级谱图库检索的方式,实现了中华鳖中42种兽药快速定性确证。应用所建立的方法对28个中华鳖样品进行筛查,共检出3种兽药残留。该方法操作简便、结果准确,适用于中华鳖中多种兽药的快速筛查分析。

    Abstract:

    In this study, a liquid chromatography combined with quadrupole/time-of-flight mass spectrometry (LC-Q-TOF/MS) was tested for the screening of about 42 veterinary drugs in Chinese softshell turtle. The sample was treated with acetonitrile and water (6∶4, V/V) to remove protein and fat, and then the supernatant was concentrated and cleaned with solid-phase extraction (SPE) system (HLB column). The veterinary drugs in the prepared sample were qualitatively and quantitatively analyzed by LC-Q-TOF/MS in positive ionization mode within 10 min. The linear ranges of the veterinary drugs were with good linearity, and the limits of detection (LOD) were from 5 to 50 μg/kg. At the different spiked levels, the average recoveries were from 56.8% to 103.8%, and the relative standard deviations (RSD) ranged from 1.26% to 10.01%. Rapid screening and confirmation of the 42 veterinary drugs can be achieved with accurate mass database and second-order spectrum library search. The method has been applied to 28 Chinese softshell turtle samples, and 3 kinds of veterinary drugs were detected. This proposed method was convenient, reliable and simple, and also was suitable for the high-throughput and rapid screening analysis of veterinary drugs in Chinese softshell turtle.

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李诗言,张海琪, 郑重莺,等.高效液相色谱-四极杆-飞行时间质谱法筛查中华鳖中42种兽药残留[J].中国渔业质量与标准,2015,5(1):42-51. LI Shiyan, ZHANG Haiqi, ZHENG Chongying, et al. Rapid screening and confirmation of 42 veterinary drugs in Chinese softshell turtle by liquid chromatography/quadrupole time-of-flight mass spectrometry[J]. Chinese Fishery Quality and Standards,2015,5(1):42-51.

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  • 最后修改日期:2017-04-26
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