超高压液相色谱串联高分辨质谱筛查渔用投入品中禁限用药物

引用本文: 孔聪, 周哲, 汪洋, 黄原飞, 沈晓盛, 黄冬梅, 蔡友琼, 于慧娟. 超高压液相色谱串联高分辨质谱筛查渔用投入品中禁限用药物[J]. 分析化学, 2017, 45(2): 245-252. doi: 10.11895/j.issn.0253-3820.160653 shu

Citation: KONG Cong, ZHOU Zhe, WANG Yang, HUANG Yuan-Fei, SHEN Xiao-Sheng, Dong-Mei, CAI You-Qiong, YU Hui-Juan. Screening of Chemical Drugs in Fishery Inputs by Ultrahigh Performance Liquid Chromatography-Orbitrap High Resolution Mass spectroscopy[J]. Chinese Journal of Analytical Chemistry, 2017, 45(2): 245-252. doi: 10.11895/j.issn.0253-3820.160653 shu

超高压液相色谱串联高分辨质谱筛查渔用投入品中禁限用药物

孔聪 ^1, ,
周哲 ^2, ,
汪洋 ^1, ,
黄原飞 ^1, ,
沈晓盛 ^1, ,
黄冬梅 ^1, ,
蔡友琼 ^1, ,
于慧娟 ^1,

1.
东海水产研究所水产品质量安全与加工实验室, 上海 200090;
2.
赛默飞世尔科技(中国)有限公司, 上海 201206
基金项目:
本文系上海市农业科学委员会（沪农科推字（2016）第1-4-1号）和中央级公益性科研院所基本科研业务费专项资金（中国水产科学研究院东海水产研究所）（No.2014T05）、上海市科学技术委员会扬帆人才计划项目（No.14YF1408100）资助。

摘要: 建立了超高压液相色谱-静电场轨道离子阱质谱系统对渔用投入品中可能造成风险隐患的禁限用药物的快速筛查与定量技术。以水（含1%甲酸）-乙腈（1∶9，V/V）溶液进行提取，通过稀释降低基质效应，在Accucore RP-MS色谱柱（100 mm×2.1 mm，2.6 μm）上，以水（含0.1%甲酸）和乙腈（含0.1%甲酸）溶液为流动相，利用梯度洗脱、HESI离子化，Full-scan ddMS2（TopN）扫描模式进行数据采集，通过与预先建立好的药物标准品质谱、色谱数据库进行比对分析，实现了53种禁限用药同时筛查确证与定量分析。各药物最低检出浓度均低于10 ng/mL，在0.01~1.0 μg/mL范围内，各药物的线性相关系数均大于0.98，根据实际测定结果设定对渔药及渔用饲料中筛查药物的检出限分别为0.5和5.0 mg/L，对渔药及渔用饲料基质添加10和100 mg/kg的各筛查成分，定量回收率均高于50%，相对标准偏差均小于15%。将本方法用于农业部渔用投入品质量安全隐患排查项目中，共筛查68个样品，其中在29个渔用兽药样品中筛查出15种说明书中未标明成分。

关键词:

English

Screening of Chemical Drugs in Fishery Inputs by Ultrahigh Performance Liquid Chromatography-Orbitrap High Resolution Mass spectroscopy

1.
East China Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences, Shanghai 200090, China;
2.
Thermo Fisher Scientific Incorporation, Shanghai 201206, China
Received Date: 03 September 2016
Revised Date: 05 December 2016

Abstract: To screen the illegal substances in fishery inputs, we established the database including the precursor and the daughter ions for these possible components by the quadrupole/orbit-trap mass spectrometer, and the retention time of each drug on the same chromatographic column. And then, the extracted and diluted samples were analyzed and the components in the real samples were identified under the same conditions. Chromatographic analysis was performed on an Accucore RP-MS column (100 mm×2.1 mm, 2.6 μm) using gradient elution with 0.1% formic acid in water and 0.1% formic acid in acetonitrile as mobile phase. Elutes were ionized through heatable electrospray ionization (HESI) in both positive and negative mode simultaneously. Data acquisition was conducted by Full-scan ddMS2 (TopN) mode, in which the full mass profile for a continuous precursor ion injection and the fragments of each high abundant precursor of targeted were acquired with excellent time and mass resolution. Screening was carried out through comparison of the information of real samples with that of standards in the database, which were processed by software (Tracefinder). The Quantification of each component was analyzed based on the precursor ion chromatography acquired by orbit-trap mass spectroscopy, which showed a good linearity between 0.01-1 μg/mL, with R>0.98. The method was validated by checking its minimum screening concentration (0.5 mg/L for drugs and 5 mg/L for feedstuffs) and evaluating the recovery after addition of the standard mixture in real samples (>50%, under the addition of 10 and 100 mg/kg). The results for 68 practical samples demonstrated the effective performance of this method for screening with high-throughput, rapidness and acceptable minimum screening concentration and accuracy, in which 15 of 29 fishery drug samples were screened out for positive components that were not indicated in their labels.

Key words:

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沈阳化工大学材料科学与工程学院沈阳 110142

超高压液相色谱串联高分辨质谱筛查渔用投入品中禁限用药物

English

Screening of Chemical Drugs in Fishery Inputs by Ultrahigh Performance Liquid Chromatography-Orbitrap High Resolution Mass spectroscopy

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中国化学会秘书处

超高压液相色谱串联高分辨质谱筛查渔用投入品中禁限用药物

English

Screening of Chemical Drugs in Fishery Inputs by Ultrahigh Performance Liquid Chromatography-Orbitrap High Resolution Mass spectroscopy

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

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CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

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CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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