超高效液相色谱-四极杆飞行时间质谱法测定克氏螯虾中39种兽药残留

doi:10.3724/SP.J.1123.2018.08037

色谱 ›› 2018, Vol. 36 ›› Issue (12): 1261-1268.DOI: 10.3724/SP.J.1123.2018.08037

超高效液相色谱-四极杆飞行时间质谱法测定克氏螯虾中39种兽药残留

宋伟^1,2, 赵暮雨¹, 韩芳^1,2, 吕亚宁^1,2, 丁磊¹, 周典兵¹, 邓晓军³, 胡艳云^1,2, 郑平^1,2, 盛旋¹

1. 安徽出入境检验检疫局检验检疫技术中心, 安徽合肥 230022;
2. 食品安全分析与检测安徽省重点实验室, 安徽合肥 230022;
3. 上海出入境检验检疫局动植物与食品检验检疫技术中心, 上海 200135

收稿日期:2018-08-25 出版日期:2018-12-08 发布日期:2014-11-06
通讯作者: 胡艳云,E-mail:huyanyun@ahciq.gov.cn
基金资助:
安徽省公益性研究联动项目（1704f0804057）；上海市长三角科技合作项目（17395810102）.

Determination of 39 veterinary drug residues in Procambarusclarkii by ultra-high performance liquid chromatography-quadrupole-time of flight mass spectrometry

SONG Wei^1,2, ZHAO Muyu¹, HAN Fang^1,2, LÜ Yaning^1,2, DING Lei¹, ZHOU Dianbing¹, DENG Xiaojun³, HU Yanyun^1,2, ZHENG Ping^1,2, SHENG Xuan¹

1. Technical Center for Inspection and Quarantine of Anhui Entry-Exit Inspection and Quarantine Bureau, Hefei 230022 China;
2. Anhui Province Key Laboratory of Analysis and Detection for Food Safety, Hefei 230022, China;
3. Technical Center for Animal Plant and Food Inspection and Quarantine, Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China

Received:2018-08-25 Online:2018-12-08 Published:2014-11-06
Supported by:
Linkage Research Project for Public Welfare in Anhui (No. 1704f0804057); Science and Technology Cooperation Project of Yangtze River Delta in Shanghai (No. 17395810102).

摘要/Abstract

摘要：

建立了超高效液相色谱-四极杆飞行时间质谱（UHPLC-Q-TOF-MS）快速筛查克氏螯虾中39种兽药残留的分析方法。样品经酸化乙腈提取，增强型脂质去除净化剂（EMR-Lipid）结合石墨化多壁碳纳米管（GMWNTs）净化，采用UHPLC-Q-TOF-MS分析检测。通过比对待测物准分子离子的精确质量数、同位素丰度比、保留时间等特征信息进行定性初筛，通过二级谱图谱库检索比对进行确证，通过一级提取离子色谱图峰面积进行定量分析。39种化合物在各自的浓度范围内均呈良好的线性关系，线性相关系数均大于0.99，定量限为3~15 μg/kg，添加回收率为62.4%~105.8%，相对标准偏差（RSD）为2.5%~13.5%，方法简便、快速、准确，可应用于克氏螯虾中喹诺酮类、磺胺类、三苯甲烷类39种药物残留的快速筛查定量。

关键词: 超高效液相色谱-四极杆飞行时间质谱, 克氏螯虾, 石墨化多壁碳纳米管, 兽药残留, 增强型脂质去除净化剂

Abstract:

An ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF-MS) method was developed for determination of 39 veterinary drugs in Procambarusclarkii. Samples were extracted with acidified acetonitrile and purified with enhanced matrix removal-lipid (EMR-Lipid) adsorbent and graphitized multi-walled carbon nanotubes (GMWNTs). Extracts were analyzed by UHPLC-Q-TOF-MS. Target compounds were screened according to accurate mass, isotopic ratio, and retention time, and confirmed by library search. Target analytes were quantified using the chromatographic peak area of each compound. For each of the drugs of interest, calibration curves were linear in their respective ranges with correlation coefficients greater than 0.99. The limits of quantification (LOQs) were 3-15 μg/kg. The recoveries for target compounds spiked in Procambarusclarkii ranged from 62.4% to 105.8%, with relative standard deviations (RSDs) ranging from 2.5% to 13.5%. This method is simple, rapid, accurate, and suitable for simultaneous determination of 39 veterinary drugs, including sulfonamides, quinolones, and triphenylmethane, extracted from Procambarusclarkii.

Key words: enhanced matrix removal-lipid adsorbent, graphitized multi-walled carbon nanotubes (GMWNTs), Procambarusclarkii, ultra-high performance liquid chromatography-quadrupole-time of flight mass spectrometry (UHPLC-Q-TOF-MS), veterinary drug residues

中图分类号:

O658

宋伟, 赵暮雨, 韩芳, 吕亚宁, 丁磊, 周典兵, 邓晓军, 胡艳云, 郑平, 盛旋. 超高效液相色谱-四极杆飞行时间质谱法测定克氏螯虾中39种兽药残留[J]. 色谱, 2018, 36(12): 1261-1268.

SONG Wei, ZHAO Muyu, HAN Fang, LÜ Yaning, DING Lei, ZHOU Dianbing, DENG Xiaojun, HU Yanyun, ZHENG Ping, SHENG Xuan. Determination of 39 veterinary drug residues in Procambarusclarkii by ultra-high performance liquid chromatography-quadrupole-time of flight mass spectrometry[J]. Chinese Journal of Chromatography, 2018, 36(12): 1261-1268.

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超高效液相色谱-四极杆飞行时间质谱法测定克氏螯虾中39种兽药残留

Determination of 39 veterinary drug residues in Procambarusclarkii by ultra-high performance liquid chromatography-quadrupole-time of flight mass spectrometry

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