首页|高效液相色谱串联质谱法检测水产品及其制品中沙丁胺醇残留

高效液相色谱串联质谱法检测水产品及其制品中沙丁胺醇残留

Determination of salbutamol in aquatic products and their products by performance liquid chromatography-tandem mass spectrometry

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目的 建立水产品及其制品中沙丁胺醇残留检测的高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS).方法 样品加入乙酸铵缓冲液(pH=5.2),37℃条件下酶解过夜,乙酸乙酯-异丙醇(1:1,v/v)提取,QuEChERS净化,HPLC-MS/MS多反应监测模式检测,内标法定量.结果 沙丁胺醇的测定低限为 0.5µg/kg,在 0.5、1.0、5.0µg/kg 3 个浓度添加水平,总体平均回收率在 87.8%~110.7%范围内,相对标准偏差为 2.7%~9.6%.结论 该方法操作简单,灵敏度、精密度、回收率均满足残留检测法规要求,精准解决了目前水产品制品中沙丁胺醇药物残留监控没有相关技术支撑的难题.
Objective A method based on performance liquid chromatography-tandem mass spectrometry(LC-MS/MS)has been developed for the determination of salbutamol in aquatic products and their products.Methods The analyte was enzymatic hydrolyzed in NH4AC solution overnight at 37℃,and extracted by ethyl acetate-isopropanol(1:1,v/v).The extract was cleaned up by QuEChERS method.Quantification was achieved by HPLC-MS/MS with multiple reaction monitoring(MRM)using internal standard method.Results The limit of quantification of salbutamol was 0.5 µg/kg.The average recoveries at three spiked levels of 0.5,1.0 and 5.0 µg/kg ranged from 87.8%to 110.7%with the relative standard deviations of 2.7%~9.6%(n=6).Conclusion The method has the advantages of simple pretreatment steps and its sensitivity,precision,and recoveries all meet the requirements of residue detection regulations,accurately solving the problem of lack of relevant technical support for monitoring salbutamol residues in aquatic products and their products.

aquatic products and their productssalbutamolhigh performance liquid chromatography-tandem mass spectrometry

王凤美、韩静静、张晓梅、张鸿伟、何京澄

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青岛海关技术中心,青岛 266109

水产品及其制品 沙丁胺醇 高效液相色谱-串联质谱

青岛海关科技攻关计划

QK202203

2024

实验室检验
中国检验检测学会

实验室检验

ISSN:2097-261X
年,卷(期):2024.2(2)
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