食品与发酵工业 >

2021 , Vol. 47 >Issue 23: 240 - 245

DOI: https://doi.org/10.13995/j.cnki.11-1802/ts.024850

分析与检测

RRLC-MS/MS法测定酒类产品中11种非法添加利尿组分

  • 王超 ,
  • 刘小芳 ,
  • 徐慧 ,
  • 杨钊
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  • 1(青岛市食品药品检验研究院,山东 青岛,266071)
    2(中国水产科学研究院 黄海水产研究所,农业农村部极地渔业开发重点实验室,山东 青岛,266071)
硕士研究生,工程师(杨钊主任药师为通讯作者,E-mail:yangzhaosyy@qd.shandong.cn)

收稿日期: 2020-06-29

  修回日期: 2020-07-29

  网络出版日期: 2021-12-31

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Determination of diuretics in alcoholic products by RRLC-MS/MS

  • WANG Chao ,
  • LIU Xiaofang ,
  • XU Hui ,
  • YANG Zhao
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  • 1(Qingdao Institute for Food and Drug Control,Qingdao 266071,China)
    2(Yellow Sea Fisheries Research Institute,Chinese Academy of Fishery Sciences,Key Laboratory of Sustainable Development of Polar Fishery,Ministry of Agriculture and Rural Affairs,Qingdao 266071,China)

Received date: 2020-06-29

  Revised date: 2020-07-29

  Online published: 2021-12-31

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摘要

旨在建立同时测定酒类产品中11种非法添加利尿组分的快速分离液相色谱-质谱联用(rapid resolution liquid chromatography-mass spectrometry,RRLC-MS/MS)方法,为酒类产品中非法添加利尿组分的监督检查和预防筛查提供技术支持。样品经甲醇溶解,上机前以甲醇-水(体积比9∶1)稀释,过滤,采用Agilent ZORBAX Eclipse plus C18 Rapid Resolution HD(3.0 mm×50 mm,1.8 μm)色谱柱进行分离,以0.1%(体积分数)的甲酸溶液和含0.1%(体积分数)甲酸的甲醇作为流动相进行梯度洗脱。质谱选用AJS ESI源,正负模式同扫,动态多反应监测(multiple reaction monitoring,MRM)模式。实验以目标离子对的保留时间和离子比率进行定性分析,以定量离子对的峰面积通过外标法进行定量分析。结果表明,11种化合物在实验的线性范围内均具有良好的相关性,相关系数均大于0.999 0;检出限为0.8~133.9 ng/g;定量限为2.7~446.3 ng/g;6份样品加标平均回收率为88.3%~105.3%,平均相对标准偏差(relative standard deviation,RSD)为0.3%~2.2%。实验所建立的方法操作简便、筛查效率高,具有较好的方法专属性和较高的灵敏度,适用于酒类产品中11种非法添加利尿组分的定性筛查和定量分析。

关键词： 酒; 利尿组分; 快速液相色谱-串联四级杆质谱; 动态多反应监测

本文引用格式

王超 , 刘小芳 , 徐慧 , 杨钊 . RRLC-MS/MS法测定酒类产品中11种非法添加利尿组分[J]. 食品与发酵工业, 2021 , 47(23) : 240 -245 . DOI: 10.13995/j.cnki.11-1802/ts.024850

Abstract

Rapid resolution liquid chromatography-mass spectrometry (RRLC-MS/MS) was established for determination of diuretics in alcoholic products. The target compounds were identified with retention time and ion ratio and quantified with area of quantitative ion by external standard method (ESTD). The results showed that RRLC-MS/MS exhibited well linear in the range of 0.01-0.2 μg/mL. The limits of detections and quantification were in the range of 0.8-133.9 ng/g and 2.7-446.3 ng/g, respectively. The mean recoveries of six samples were 88.3%-105.3% with the relative standard deviations from 0.3% to 2.2%. RRLC-MS/MS can provide scientific knowledge for the regulation and prevention of alcoholic products.

Key words： alcoholic products; diuretics; RRLC-MS/MS; dynamic MRM

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