Development of a Method for the Rapid Determination of 17 Veterinary Drug Residues in Foods of Animal Origin by UPLC-MS/MS Combined with Pass-Through SPE Cartridge

IF 2.6 3区农林科学 Q2 FOOD SCIENCE & TECHNOLOGY

Food Analytical Methods Pub Date : 2024-11-16 DOI:10.1007/s12161-024-02712-8

Qianran Sun, Jun Liu, Yuan Gou, Wei Dong, Tao Wang, Huidan Deng, Yi Hua, Yicheng Shi

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Abstract

In this study, a method was developed for the rapid determination of 17 veterinary drug residues in foods of animal origin using pass-through solid-phase extraction (SPE) coupled with ultra–high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Two grams of the sample was extracted ussing 8 mL of acetonitrile to water (85:15). An Oasis® HLB cartridge was selected for the clean-up of the sample without activation/calibration and elution. The separation was performed on an Acquity UPLC HSS T3 column (2.1 mm*100 mm, 1.8 μm) with a gradient elution using methanol–0.2% formic acid aqueous solution as the mobile phase. The analytes were detected in polarity switching electrospray ionization (ESI + / −) and multiple reaction monitoring (MRM) modes. The quantification was conducted using a matrix-matched standard solution external standard method. The performance of the employed UPLC-MS/MS method was observed to be satisfactory. The recoveries of the tests were within the range of 65.1–114.4%, with the relative standard deviations (RSDs) being lower than 12.3%. The limits of quantification (LOQs) of the target compounds ranged from 0.3 to 2.0 μg/kg (S/N ≥ 10), which complied with the relevant matrix limits mentioned in the food safety standards of Korea, the United States, and Canada in recent years. Positive samples of pentetrazol were identified in two batches of fish and one batch of chicken. However, the levels did not exceed the maximum residue level (MRL). This method has been successfully employed for the detection of a number of food products of animal origin in the local market, providing a methodological reference in cross-border food safety and testing.

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UPLC-MS/MS - Pass-Through固相萃取（SPE）快速检测动物源性食品中17种兽药残留方法的建立

本研究建立了一种动物源性食品中17种兽药残留的快速测定方法——固相萃取(SPE) -超高效液相色谱-串联质谱（UPLC-MS/MS）联用技术。用8ml乙腈对水（85:15）提取2g样品。选择Oasis®HLB滤筒进行样品清理，无需活化/校准和洗脱。采用Acquity UPLC HSS T3色谱柱（2.1 mm*100 mm, 1.8 μm），甲醇- 0.2%甲酸水溶液为流动相，梯度洗脱。分析物采用极性开关电喷雾电离（ESI + /−）和多反应监测（MRM）模式进行检测。采用矩阵匹配标准溶液外标法进行定量。所采用的UPLC-MS/MS方法的性能令人满意。加样回收率为65.1 ~ 114.4%，相对标准偏差（rsd）小于12.3%。目标化合物的定量限（loq）范围为0.3 ~ 2.0 μg/kg (S/N≥10)，符合韩国、美国、加拿大近年食品安全标准中相关基质的限量要求。在两批鱼和一批鸡中检出戊四唑阳性样品。但未超过最大残留限量（MRL）。该方法已成功应用于本地市场多个动物源性食品的检测，为跨境食品安全和检测提供了方法参考。

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来源期刊

Food Analytical Methods 农林科学-食品科技

CiteScore

6.00

自引率

3.40%

发文量

244

审稿时长

3.1 months

期刊介绍： Food Analytical Methods publishes original articles, review articles, and notes on novel and/or state-of-the-art analytical methods or issues to be solved, as well as significant improvements or interesting applications to existing methods. These include analytical technology and methodology for food microbial contaminants, food chemistry and toxicology, food quality, food authenticity and food traceability. The journal covers fundamental and specific aspects of the development, optimization, and practical implementation in routine laboratories, and validation of food analytical methods for the monitoring of food safety and quality.