食品科学 ›› 2021, Vol. 42 ›› Issue (22): 324-330.doi: 10.7506/spkx1002-6630-20200817-220

• 安全检测 • 上一篇    

超高效液相色谱-串联质谱法同时测定小麦粉中硫脲、曲酸、噻苯咪唑、噻二唑、四环素

王妍,李志刚,赵文涛,郭文萍,李莹莹,王娟强,姜锐   

  1. (中国肉类食品综合研究中心,北京 100068)
  • 发布日期:2021-11-23
  • 基金资助:
    国家重点研发计划“食品安全关键技术研发”重点专项(2017YFC1601706);北京市博士后工作经费资助项目

Simultaneous Determination of Thiourea, Kojic Acid, Thiabendazole, Thiadiazole and Tetracycline in Flour by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

WANG Yan, LI Zhigang, ZHAO Wentao, GUO Wenping, LI Yingying, WANG Juanqiang, JIANG Rui   

  1. (China Meat Food Research Center, Beijing 100068, China)
  • Published:2021-11-23

摘要: 建立超高效液相色谱-串联质谱法同时测定小麦粉中硫脲、曲酸、噻苯咪唑、噻二唑、四环素5 种非法添加物的快速定量检测方法。样品经80%乙醇溶液-乙腈(1∶1,V/V)提取、离心、氮吹浓缩后,采用多反应监测模式进行定性、定量分析。结果表明:本方法中硫脲、曲酸、四环素在100~5 000 ng/mL、噻苯咪唑在1~50 ng/mL、噻二唑在1~50 μg/mL范围内线性关系良好,相关系数大于0.999。硫脲、曲酸、四环素检出限为25 μg/kg,定量限为50 μg/kg;噻苯咪唑检出限为0.5 μg/kg,定量限为1 μg/kg;噻二唑检出限为0.5 mg/kg,定量限为1 mg/kg。基质添加回收率范围在88.6%~102.2%之间,相对标准偏差在0.7%~5.6%之间(n=6)。该方法前处理简单、快速,可用于小麦粉中硫脲、曲酸、噻苯咪唑、噻二唑、四环素5 种非法添加物的快速测定。

关键词: 小麦粉;非法添加物;液相色谱-串联质谱

Abstract: In this research, an analytical method for simultaneous determination of thiourea, kojic acid, thiabendazole, thiadiazole and tetracycline in wheat flour by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was established. Samples were extracted with 80% ethanol-acetonitrile (1:1, V/V), and then subjected to centrifugation and nitrogen blowing concentration before being quantitatively analyzed by using the multi-reaction monitoring (MRM) mode. The results showed that the developed method exhibited a good linear relationship in the concentration range of 100–5 000 ng/mL for thiourea, kojic acid and tetracycline, 1–50 ng/mL for thiabendazole and 1–50 μg/mL for thiadiazole, with correlation coefficients of higher than 0.999. The limits of detection (LOD) and limits of quantitation (LOQ) were 25 and 50 μg/kg for thiourea, kojic acid and tetracycline; 0.5 and 1 μg/kg for thiabendazole; 0.5 and 1 mg/kg for thiadiazole. The recoveries from spiked samples ranged from 88.6% to 102.2%, and the precision expressed as relative standard deviation (RSD) ranged from 0.7% to 5.6% (n = 6). This method, with simple and rapid pretreatment, can be used for the rapid determination of thiourea, kojic acid, thiabendazole, thiadiazole and tetracycline in wheat flour.

Key words: wheat flour; illegal additives; liquid chromatography-tandem mass spectrometry

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