色谱

色谱 ›› 2019, Vol. 37 ›› Issue (9): 946-954.DOI: 10.3724/SP.J.1123.2019.02016

• 研究论文 • 上一篇    下一篇

分散固相萃取净化-超高效液相色谱-串联质谱法同时测定鱼和虾中抗生素及三苯甲烷类兽药残留

陈兴连, 林涛, 刘兴勇, 梅文泉, 杨东顺, 李彦刚, 李茂萱, 汪禄祥   

  1. 1. 云南省农业科学院质量标准与检测技术研究所, 云南 昆明 650224;
    2. 农业农村部农产品质量监督检验测试中心(昆明), 云南 昆明 650224
  • 收稿日期:2019-02-28 出版日期:2019-09-08 发布日期:2015-07-30
  • 通讯作者: 汪禄祥
  • 基金资助:
    云南省科技厅科技计划项目（重大专项计划）（2018BC005-04）.

Simultaneous determination of antibiotics and triphenylmethanes veterinary drug residues in fish and shrimp by dispersive solid phase extraction purification-ultra high performance liquid chromatography-tandem mass spectrometry

CHEN Xinglian, LIN Tao, LIU Xingyong, MEI Wenquan, YANG Dongshun, LI Yangang, LI Maoxuan, WANG Luxiang   

  1. 1. Quality Standardizing and Testing Technology Institute, Yunnan Academy of Agricultural Sciences, Kunming 650224, China;
    2. Supervision & Testing Center for Farm Products Quality, Ministry of Rural Agriculture(Kunming Section), Kunming 650224, China
  • Received:2019-02-28 Online:2019-09-08 Published:2015-07-30
  • Supported by:
    Science and Technology Project of Yunnan Science and Technology Department (Major Special Project) (No. 2018BC005-04).

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摘要： 建立了分散固相萃取净化-超高效液相色谱-串联质谱法快速测定鱼和虾中3类（磺胺类、喹诺酮类、氯霉素类）18种抗生素及2种三苯甲烷类（孔雀石绿、隐色孔雀石绿）兽药残留。样品经磷酸氢二钾溶液水解分散，乙腈提取，提取液经氯化钠脱水、盐析后取乙腈层，经旋转蒸发仪浓缩至近干，残留物用甲醇定容至1.0 mL，C18和PSA（N-丙基乙二胺）填料分散固相萃取净化，过滤膜后经ZORBAX C18色谱柱（50 mm×2.1 mm，1.8 μm）分离，正、负离子多反应监测模式采集数据，同位素内标法定量。实验结果表明，20种兽药在0.2~300 μg/L范围内具有良好的线性关系，检出限为0.1~0.6 μg/kg，定量限为0.3~1.8 μg/kg，相关系数均大于0.99。在1、5和20倍定量限加标浓度水平下，平均回收率为72.5%~118%，相对标准偏差（RSD）为1.9%~9.8%。该方法具有前处理简单、检测效率高、成本低等优点，适用于鱼和虾中多类兽药残留的同时测定。

关键词: 超高效液相色谱, 串联质谱法, 分散固相萃取, 抗生素, 三苯甲烷类, 兽药残留, 虾, 鱼

Abstract: A method was established to rapidly determine 20 kinds of veterinary drug residues including three catagories of antibiotics (sulfonamides, quinolones, and chloramphenicols) and two kinds of triphenylmethanes (malachite green (MG) and leucomalachite green (LMG)) in fish and shrimp, based on dispersive solid phase extraction purification-ultra high performance liquid chromatography-tandem mass spectrometry. The samples were first hydrolyzed using a dipotassium hydrogen phosphate solution, and then extracted using acetonitrile. Afterward, the extraction solution was dehydrated and salted out with sodium chloride and condensed to nearly dry using a rotating evaporator. This residue was dissolved in 1.0 mL methanol. The resulting solution was purified by dispersive solid phase extraction method with C18 and PSA sorbents, and filtered through a filter. The target compounds were separated employing a ZORBAX C18 column. The mass spectrometer datas were acquired by multiple reaction monitoring (MRM) of positive and negative modes and quantitated applying the isotope internal standard method. The 20 veterinary drugs showed a good linear relationship in the range of 0.2-300 μg/L. The limits of detection and the limits of quantification were 0.1-0.6 and 0.3-1.8 μg/kg, respectively, while the correlation coefficients were greater than 0.99. The average recoveries at the three spiked levels (1, 5, and 20 times of quantitative limits) ranged between 72.5%-118%, with the relative standard deviations of 1.9%-9.8%. The advantages of method include a simple pretreatment, a high detection efficiency, and a low cost. Moreover, it is suitable for the simultaneous determination of multiple veterinary drug residues in fish and shrimp.

Key words: antibiotics, dispersive solid phase extraction (DSPE), fish, shrimp, tandem mass spectrometry (MS/MS), triphenylmethanes, ultra high performance liquid chromatography (UHPLC), veterinary drug residue

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