亲水作用色谱-串联质谱法检测畜禽肝脏和肾脏中氨基糖苷类药物残留

doi:10.7506/spkx1002-6630-20241212-094

食品科学 ›› 2025, Vol. 46 ›› Issue (11): 320-326.doi: 10.7506/spkx1002-6630-20241212-094

• 安全检测 • 上一篇

亲水作用色谱-串联质谱法检测畜禽肝脏和肾脏中氨基糖苷类药物残留

薛霞，魏莉莉，王骏，宿书芳，公丕学，张艳侠，倪来学，姚现琦，万宇平，刘艳明

（1.山东省食品药品检验研究院，国家市场监管重点实验室（肉及肉制品监管技术），产业技术基础公共服务平台，山东济南 250101；2.临沂金锣文瑞食品有限公司，山东临沂 276000；3.北京勤邦科技股份有限公司，北京 102206）

发布日期:2025-05-14
基金资助:
北京市科技计划项目（Z221100007122001）；国家市场监督管理总局科技计划项目（2022MK072）

Hydrophilic Interaction Chromatography-Tandem Mass Spectrometry for Determination of Aminoglycoside Residues in Liver and Kidney Samples from Livestock and Poultry

XUE Xia, WEI Lili, WANG Jun, SU Shufang, GONG Peixue, ZHANG Yanxia, NI Laixue, YAO Xianqi, WAN Yuping, LIU Yanming

(1. Key Laboratory of Supervising Technology for Meat and Meat Products for State Market Regulation, Industrial Technology Foundation Public Service Platform, Shandong Institute for Food and Drug Control, Jinan 250101, China; 2. Linyi Jinluo WinRay Food Co. Ltd., Linyi 276000, China; 3. Beijing Kwinbon Technology Co. Ltd., Beijing 102206, China)

Published:2025-05-14

摘要/Abstract

摘要： 针对畜禽肝脏和肾脏中氨基糖苷类药物残留检测的难题，改进提取溶剂和净化方法，建立基于亲水作用色谱-串联质谱的分析技术，可实现12 种氨基糖苷类药物的快速、准确测定。方法以磷酸盐缓冲溶液（含50 g/L三氯乙酸和50 g/L氯化钠）作为提取溶剂，显著提高了新霉素的回收率；提取液经适当稀释后，PRiME HLB固相萃取柱进行净化，混合型两性离子键合亲水作用色谱柱分离，使用含有1.0%甲酸水（甲酸铵浓度为1 mmol/L）和乙腈作为流动相的梯度洗脱方法，利用超高效液相色谱-串联质谱仪进行分析测定。安普霉素、潮霉素B、新霉素和妥布霉素采用内标法定量，其余化合物采用外标法定量。结果表明，12 种目标物在指定的浓度范围内显示出良好的线性响应，决定系数均≥0.99。检出限为10～50 μg/kg，定量限为20～100 μg/kg。在8 种空白肝脏和肾脏基质中进行低、中、高3 个水平的加标回收实验（n＝6），各药物的回收率在78.0%～108.5%之间，相对标准偏差在1.0%～11.0%之间。本方法采用单一固相萃取柱净化，操作简便，适用于畜禽肝脏和肾脏中氨基糖苷类药物残留的准确定性与定量分析。

关键词: 氨基糖苷类药物；PRiME?HLB固相萃取柱；肝脏；肾脏；亲水作用色谱-串联质谱法

Abstract: To address the difficulty of detecting aminoglycoside (AG) residues in the liver and kidney of livestock and poultry, the extraction solvent and purification method were improved. A rapid and accurate method for the determination of 12 AGs was developed using hydrophilic interaction chromatography-tandem mass spectrometry (HIC-MS/MS). This method employed phosphate buffer solution containing 50 g/L trichloroacetic acid and 50 g/L sodium chloride as the extraction solvent, which significantly improved the recovery of neomycin. After proper dilution, the extract was purified on a PRiME HLB solid phase extraction (SPE) column. Subsequently, the chromatographic separation was performed on an Obelisc R column using gradient elution with a mobile phase composed of acetonitrile and 1.0% formic acid in water (containing 1 mmol/L ammonium formate) before analysis by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The internal standard method was used for the quantitation of apramycin, hygromycin B, neomycin, and tobramycin, while the external standard method was adopted for the quantitation of the remaining eight compounds. The results revealed that the calibration curves for all analytes had good linearity within the corresponding concentration ranges, with determination coefficients of ≥ 0.99. The limits of detection (LOD) and quantitation (LOQ) ranged from 10 to 50 μg/kg and from 20 to 100 μg/kg, respectively. The recoveries for 8 blank liver and kidney matrices at low, medium, and high spiked levels were 78.0%–108.5%, with relative standard deviations (RSDs) ranging from 1.0% to 11.0% (n = 6). Using a single solid-phase extraction cartridge, the method developed herein is simple and easy to operate and can be used for accurate qualitative and quantitative analysis of AG residues in liver and kidney samples.

Key words: aminoglycosides; PRiME HLB solid phase extraction cartridge; liver; kidney; hydrophilic interaction chromatography-tandem mass spectrometry

中图分类号:

O657.7

薛霞，魏莉莉，王骏，宿书芳，公丕学，张艳侠，倪来学，姚现琦，万宇平，刘艳明. 亲水作用色谱-串联质谱法检测畜禽肝脏和肾脏中氨基糖苷类药物残留[J]. 食品科学, 2025, 46(11): 320-326.

XUE Xia, WEI Lili, WANG Jun, SU Shufang, GONG Peixue, ZHANG Yanxia, NI Laixue, YAO Xianqi, WAN Yuping, LIU Yanming. Hydrophilic Interaction Chromatography-Tandem Mass Spectrometry for Determination of Aminoglycoside Residues in Liver and Kidney Samples from Livestock and Poultry[J]. FOOD SCIENCE, 2025, 46(11): 320-326.

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亲水作用色谱-串联质谱法检测畜禽肝脏和肾脏中氨基糖苷类药物残留

Hydrophilic Interaction Chromatography-Tandem Mass Spectrometry for Determination of Aminoglycoside Residues in Liver and Kidney Samples from Livestock and Poultry

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