通过式固相萃取结合超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速筛查畜禽肉中108种兽药残留

引用本文: 郭添荣, 万渝平, 孙利, 叶梅, 许森, 韩世鹤, 吴文林. 通过式固相萃取结合超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速筛查畜禽肉中108种兽药残留[J]. 分析化学, 2022, 50(2): 271-277. doi: 10.19756/j.issn.0253-3820.211059 shu

Citation: GUO Tian-Rong, WAN Yu-Ping, SUN Li, YE Mei, XU Sen, HAN Shi-He, WU Wen-Lin. Rapid Screening and Confirmation of 108 Kinds of Veterinary Drug Residues in Livestock and Poultry Meat by Solid Phase Extraction Purification and Liquid Chromatography Coupled with Quadrupole/Orbitrap Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2022, 50(2): 271-277. doi: 10.19756/j.issn.0253-3820.211059 shu

通过式固相萃取结合超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速筛查畜禽肉中108种兽药残留

郭添荣 ^1, ,
万渝平 ^1, ,
孙利 ^2, ,
叶梅 ^1, ,
许森 ^3, ,
韩世鹤 ^{2,
,} ,
吴文林 ^{1,4,
,}

1.
成都市食品检验研究院,成都 611130;
2.
中国检验检疫科学研究院,北京 100176;
3.
华东理工大学上海市功能性材料化学重点实验室,上海 200237;
4.
中国科学院成都生物研究所,成都 610041

通讯作者: 韩世鹤,E-mail:wwl2008802@gmail.com; 吴文林,E-mail:hanshihe@hotmail.com

基金项目:
国家市场监督管理总局技术保障专项项目（No.2021YJ009）、四川省科技计划应用基础研究项目（No.21YYJC0962）和成都市技术创新研发项目（No.2021-YF05-00811-SN）资助

摘要: 采用通过式固相萃取消减样品中杂质干扰，基于超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UHPLC-Q/Orbitrap HRMS)联用技术建立了同时快速筛查畜禽肉中108种兽药残留的分析方法。样品匀质后，经乙腈溶液(80%，V/V，含0.2%甲酸)提取，Oasis PRiME HLB固相萃取柱通过式净化，氮吹后复溶。采用Agilent Eclipse plus C₁₈色谱柱(150 mm×3.0 mm, 1.8 μm)分离，以乙腈和20 mmol/L乙酸铵溶液(含0.1%甲酸)体系为流动相进行梯度洗脱，加热电喷雾离子源正负离子同时扫描模式，一级全扫描/数据依赖二级扫描(Full MS/dd-MS²)监测模式检测，基质匹配标准曲线法定量。结果表明，108种兽药在0.5～2000 ng/mL范围内线性关系良好，相关系数(R)≥0.9950；方法检出限(LOD)为0.1～20 μg/kg，定量限(LOQ)为0.2～100 μg/kg；不同畜禽肉在3个添加水平下(n=6)的加标回收率在68.7%～112.5%之间，相对标准偏差(RSD)在0.9%～9.7%之间。本方法简便快捷、覆盖目标物广、通量高且准确可靠，适用于畜禽肉中兽药多残留的快速筛查与确证分析。

关键词:

English

Rapid Screening and Confirmation of 108 Kinds of Veterinary Drug Residues in Livestock and Poultry Meat by Solid Phase Extraction Purification and Liquid Chromatography Coupled with Quadrupole/Orbitrap Mass Spectrometry

GUO Tian-Rong ^1, ,
WAN Yu-Ping ^1, ,
SUN Li ^2, ,
YE Mei ^1, ,
XU Sen ^3, ,
HAN Shi-He ^{2,
,} ,
WU Wen-Lin ^{1,4,
,}

1.
Chengdu Institute of Food Inspection, Chengdu 611130, China;
2.
Chinese Academy of Inspection and Quarantine, Beijing 100176, China;
3.
Shanghai Key Laboratory of Functional Materials Chemistry, East China University of Science and Technology, Shanghai 200237, China;
4.
Chengdu Institute of Biology, Chinese Academy of Sciences, Chengdu 610041, China

Corresponding author: HAN Shi-He, ; WU Wen-Lin,

Received Date: 23 January 2021
Revised Date: 12 November 2021
Fund Project:
Supported by the State Administration for Market Regulation, China (No.2021YJ009), the Application Basic Research Project of Science and Technology Plan of Sichuan Province, China (No.21YYJC0962) and the Technology Innovation Research and Development Project of Chengdu, China (No.2021-YF05-00811-SN)

Abstract: An analytical strategy for simultaneous and rapid screening of 108 kinds of veterinary drug residues in livestock and poultry meat was established by using solid-phase extraction (SPE) to reduce impurity interference in samples and based on ultra-high performance liquid chromatography-quadrupole/orbitrap high resolution mass spectrometry (UHPLC-Q/Orbitrap HRMS). The homogenized samples were extracted by 80% acetonitrile aqueous solution (containing 0.2% formic acid), purified by Oasis PRiME HLB solid phase extraction column, and redissolved by nitrogen blowing. The target analytes were separated from the samples by an Agilent Eclipse plus C₁₈ (3.0 mm×150 mm, 1.8 μm) chromatographic column, with acetonitrile and 0.1% acetic acid-ammonium formate (20 mmol/L) aqueous solution system as the mobile phase in gradient elution. Under the heated electrospray ionization positive and negative ions simultaneous scan mode, the target analytes were analyzed by the full scan of primary mass spectrometry plus data-dependent secondary mass spectrometry (Full MS/dd-MS²), and quantitatively detected by a matrix matching quantitative standard curve method. The results showed that 108 kinds of veterinary drugs had a good linear relationship in the range of 0.5-2000 ng/mL, and the correlation coefficients (R) were over 0.9950. The limits of detection (LODs) were 0.1-20 μg/kg, and the limits of quantitation (LOQs) were 0.2-100 μg/kg. The standard recoveries of different livestock and poultry meat under three levels of addition (n=6) were 68.7%-112.5%, and the relative standard deviation (RSDs) were 0.9%-9.7%. This method was simple, rapid and accurate, with wide coverage and high-throughput, and was suitable for rapid screening and confirmative analysis of veterinary drug residues in livestock and poultry meat.

Key words:

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

通过式固相萃取结合超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速筛查畜禽肉中108种兽药残留

通讯作者: 韩世鹤,E-mail:wwl2008802@gmail.com; 吴文林,E-mail:hanshihe@hotmail.com

English

Rapid Screening and Confirmation of 108 Kinds of Veterinary Drug Residues in Livestock and Poultry Meat by Solid Phase Extraction Purification and Liquid Chromatography Coupled with Quadrupole/Orbitrap Mass Spectrometry

Corresponding author: HAN Shi-He, ; WU Wen-Lin,

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

通过式固相萃取结合超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速筛查畜禽肉中108种兽药残留

通讯作者: 韩世鹤,E-mail:wwl2008802@gmail.com; 吴文林,E-mail:hanshihe@hotmail.com

English

Rapid Screening and Confirmation of 108 Kinds of Veterinary Drug Residues in Livestock and Poultry Meat by Solid Phase Extraction Purification and Liquid Chromatography Coupled with Quadrupole/Orbitrap Mass Spectrometry

Corresponding author: HAN Shi-He, ; WU Wen-Lin,

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

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

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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通讯作者: 陈斌, bchen63@163.com

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