免疫亲和固相萃取­液相色谱串联质谱测定乳制品中的11种氨基糖苷类药物
作者:
作者单位:

1.中国医科大学公共卫生学院, 辽宁 沈阳 110001;2.北京市疾病预防控制中心 食物中毒诊断溯源技术北京市重点实验室,北京 100013;3.内蒙古伊利事业 集团有限公司质量部,内蒙古 呼和浩特 010080

作者简介:

刘育形 女 硕士生 研究方向为营养与食品卫生 E-mail: 473488566@qq.com

通讯作者:

张晶 女 副研究员 研究方向为食品检测 E­mail: brightjing@163.com

中图分类号:

R155

基金项目:

国家重点研发计划(2017YFC1601605)


Determination of 11 aminoglycosides residues in dairy products by liquid chromatography tandem mass spectrometry after immunoaffinity SPE
Author:
Affiliation:

1.School of Public Health, China Medical University, Liaoning Shenyang 110001, China;2.Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning, Beijing Center for Disease Control and Prevention, Beijing 100013, China;3.Inner Mongolia Yili Industrial Group Co. Ltd., Inner Mongolia Hohhot 010080, China

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    摘要:

    目的 建立液奶和乳粉中11种氨基糖苷类药物(壮观霉素、双氢链霉素、潮霉素B、链霉素、庆大霉素C1、阿米卡星、庆大霉素C2、卡那霉素、庆大霉素C1a、妥布霉素和安普霉素)残留的高效液相色谱串联质谱(HPLC-MS/MS)检测方法。方法 乳制品样品经1%乙酸水溶液提取、免疫亲和小柱富集净化,5%甲酸乙腈洗脱后用HPLC-MS/MS法进行测定,乙腈和0.5%甲酸水为流动相,BEH Amide色谱柱分离,基质匹配曲线法定量分析。结果 11种氨基糖苷类抗生素在5~500 μg/L浓度范围内具有良好的线性关系,相关系数(r)均大于0.99;液奶和奶粉中目标药物的定量限分别为3和10 μg/kg;平均回收率范围为65.12%~105.95%, 相对标准偏差(RSD)为0.85%~19.12%。结论 该方法操作简单,具有良好的选择性、灵敏度和重现性,可用于乳制品中11种氨基糖苷类药物的同时检测。

    Abstract:

    Objective To establish a method for simultaneous determination of 11 aminoglycosides antibiotics (spectinomycin, dihydrostreptomycin, hygromycin B, streptomycin, gentamicin C1, amikacin, gentamicin C2, kanamycin, gentamicin C1a, tobramycin and apramycin) in liquid milk and milk powder samples by high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS).Methods The dairy products were extracted by water containing 1% acetic acid, concentrated and purified by the immunoaffinity cartridges, and then analyzed by HPLC-MS/MS. A BEH Amide column was used for the separation of target drugs as well as acetonitrile and water containing 0.5% formic aid used as the mobile phase. Matrix matched calibration was applied in the quantitation.Results The calibration curves achieved good linearity in the range of 5-500 μg/L with the correlation coefficients (r) greater than 0.99; the quantification limits of AGs in liquid milk and powder were 3 and 10 μg/kg, respectively. The average recovery ranged from 65.12% to 105.95% with relative standard deviations (RSD) ranged from 0.85% to 19.12%.Conclusion This method presented good selectivity, high sensitivity and simple operation, which was suitable for the determination of 11 aminoglycoside antibiotics in dairy products.

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刘育形,白艳梅,谢瑞龙,陈容,张晶,杨奕,李翠枝.免疫亲和固相萃取­液相色谱串联质谱测定乳制品中的11种氨基糖苷类药物[J].中国食品卫生杂志,2022,34(2):240-246.

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  • 收稿日期:2021-10-08
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  • 在线发布日期: 2022-05-18
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