食品与发酵工业 >

2022 , Vol. 48 >Issue 2: 254 - 259

DOI: https://doi.org/10.13995/j.cnki.11-1802/ts.027116

分析与检测

QuEChERS/超高效液相色谱-串联质谱法测定大黄鱼中非法染料硫代黄素

  • 赵慧男 ,
  • 郑文静 ,
  • 孙珊珊 ,
  • 王明栋 ,
  • 薛霞 ,
  • 王骏 ,
  • 祝建华 ,
  • 刘艳明 ,
  • 张艳侠
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  • 1(山东省食品药品检验研究院,山东 济南,250101)
    2(山东省食品药品安全检测工程技术研究中心,山东 济南,250101)
硕士,工程师(刘艳明研究员和张艳侠高级工程师为共同通信作者,E-mail:msymliu@163.com;zyx5560@126.com)

收稿日期: 2021-02-22

  修回日期: 2021-05-26

  网络出版日期: 2022-02-28

基金资助

国家重点研发计划(2017YFC1601600)

收起

Determination of illegal dyes thioflavine T in Larimichthys crocea by QuEChERS-UPLC-MS/MS

  • ZHAO Huinan ,
  • ZHENG Wenjing ,
  • SUN Shanshan ,
  • WANG Mingdong ,
  • XUE Xia ,
  • WANG Jun ,
  • ZHU Jianhua ,
  • LIU Yanming ,
  • ZHANG Yanxia
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  • 1(Shandong Institute for Food and Drug Control, Jinan 250101, China)
    2(Shandong Research Center of Engineering and Technology for Safety Inspection of Food and Drug, Jinan 250101, China)

Received date: 2021-02-22

  Revised date: 2021-05-26

  Online published: 2022-02-28

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摘要

建立了超高效液相色谱-串联质谱法测定大黄鱼中硫代黄素残留的分析方法。样品中的硫代黄素经乙腈-水溶液提取,QuEChERS方法净化,C18色谱柱分离,以0.1%(体积分数)甲酸水溶液-乙腈为流动相进行梯度洗脱,三重四极杆质谱电喷雾多反应监测模式检测,外标法定量。结果表明,硫代黄素为0.5~50.0 ng/mL时线性关系良好,相关系数(r)大于0.998,检出限为2.0 μg/kg,定量限为5.0 μg/kg。在5.0、20.0、100.0 μg/kg 3个浓度下的平均回收率为94.1%~99.2%,相对标准偏差小于1.60%。该方法操作简单、准确性高、重复性好,可用于大黄鱼中非法染料硫代黄素的测定,为大黄鱼的质量监管提供了有力的技术支撑。

关键词： 大黄鱼; 硫代黄素; QuEChERS; 超高效液相色谱-串联质谱法

本文引用格式

赵慧男 , 郑文静 , 孙珊珊 , 王明栋 , 薛霞 , 王骏 , 祝建华 , 刘艳明 , 张艳侠 . QuEChERS/超高效液相色谱-串联质谱法测定大黄鱼中非法染料硫代黄素[J]. 食品与发酵工业, 2022 , 48(2) : 254 -259 . DOI: 10.13995/j.cnki.11-1802/ts.027116

Abstract

An analytical method was developed for the determination of thioflavine T in Larimichthys crocea using ultra- performance liquid chromatography-tandem mass spectrometry. The samples were extracted with an acetonitrile-water solution and purified by the quick, easy, cheap, effective, rugged and safe (QuEChERS) method. The separation was carried out on a C18 column with gradient elution using 0.1% (V/V) formic acid aqueous solution and acetonitrile as mobile phases by ultra-performance liquid chromatography (UPLC). The target compound was detected by MS/MS system with electrospray ionization (ESI) under multiple reaction monitoring (MRM) mode with external standard method. Under the optimal conditions, thioflavine T showed good linearity (r>0.998) in the range of 0.5-50.0 ng/mL. The limit of detection (LOD) of the method was 2.0 μg/kg and the limit of quantitation (LOQ) was 5.0 μg/kg. Moreover, the spiked recoveries of the analyte from blank Larimichthys crocea samples at the three levels of 5.0, 20.0 and 100.0 μg/kg were in the range of 94.1%-99.2% with the relative standard deviations (RSD) less than 1.60%. With the advantage of convenience, fast, sensitivity and good repeatability, the method is suitable for the detection of thioflavine T in Larimichthys crocea.

Key words： Larimichthys crocea; thioflavine T; QuEChERS; UPLC-MS/MS

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