色谱

色谱 ›› 2014, Vol. 32 ›› Issue (1): 21-25.DOI: 10.3724/SP.J.1123.2013.07015

• 研究论文 • 上一篇    下一篇

固相萃取-液相色谱-串联质谱法测定莲蓉馅料中的二氧化硫脲

汪辉1, 曾习文2, 常晓途3, 彭新凯1, 夏立新1, 李亦蔚2   

  1. 1. 长沙市食品质量安全监督检测中心, 湖南 长沙 410013;
    2. 湖南省食品安全生产工程技术研究中心, 湖南 长沙 410013;
    3. 长沙县食品安全检测中心, 湖南 长沙 410100
  • 收稿日期:2013-07-10 修回日期:2013-08-29 出版日期:2014-01-08 发布日期:2013-12-26
  • 通讯作者: 汪辉
  • 基金资助:

    “十二五”国家科技支撑计划项目子课题(2012BAK17B17)；湖南省科技计划重点项目(2013WK2003).

Determination of thiourea dioxide in lotus seed paste fillings by solid phase extraction-liquid chromatography-tandem mass spectrometry

WANG Hui1, ZENG Xiwen2, CHANG Xiaotu3, PENG Xinkai1, XIA Lixin1, LI Yiwei2   

  1. 1. Changsha Center of Supervision and Inspection on Food Quality Safety, Changsha 410013, China;
    2. Food Safety Production Engineering Research Center of Hunan Province, Changsha 410013, China;
    3. Food Safety Inspection Center of Changsha County, Changsha 410100, China
  • Received:2013-07-10 Revised:2013-08-29 Online:2014-01-08 Published:2013-12-26

PDF

386

被引次数

6

摘要：

建立了固相萃取-液相色谱-串联质谱法测定莲蓉馅料中违法添加的二氧化硫脲的分析方法。采用0.05%(v/v)醋酸溶液从馅料中提取二氧化硫脲，经BOND ELUT PLEXA固相萃取柱(60 mg/3 mL)净化，采用Agilent亲水作用色谱柱(100 mm×2.1 mm，3.5 μm)分离，以0.01 mol/L醋酸铵(冰醋酸调pH至3.5)和乙腈为流动相，在多反应监测模式(MRM)下进行定性定量分析。最终，二氧化硫脲在10~1000 μg/L范围内线性关系良好，检出限(LOD)和定量限(LOQ)分别为8.0 μg/kg和30.0 μg/kg，方法回收率为75.3%~80.7%，相对标准偏差(n=6)不超过4.83%。此方法快速、准确、特异性强、灵敏度高、样品前处理方法简便易行，适用于莲蓉馅料中二氧化硫脲的确证与测定。

关键词: 二氧化硫脲, 固相萃取, 莲蓉馅料, 液相色谱-串联质谱

Abstract:

A method of solid phase extraction-liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) was developed to determine thiourea dioxide which was illegally added into lotus seed paste fillings. An amount of 0.05% (v/v) acetic acid was used to extract thiourea dioxide from fillings, and the BOND ELUT PLEXA column (60 mg/3 mL) was used as the SPE column to clean-up the extraction. Then, an Agilent HILIC column (100 mm×2.1 mm, 3.5 μm) was applied to separate target compounds by using the mobile phases of 0.01 mol/L ammonium acetate (pH 3.5) and acetonitrile. Qualitative and quantitative analyses were operated by the multiple reaction monitoring (MRM) mode. The calibration curve showed a good linearity for the target compound in the detection range of 10-1000 μg/L. The limit of detection (LOD) and limit of quantitation (LOQ) of this method were 8.0 μg/kg and 30.0 μg/kg, respectively. The recoveries were in the ranges of 75.3%-80.7% with the RSDs of no more than 4.83%. This proposed method was rapid, highly specific and suitable for the confirmation and quantitative determination of thiourea dioxide in lotus seed paste fillings.

Key words: liquid chromatography-tandem mass spectrometry, lotus seed paste fillings, solid phase extraction, thiourea dioxide

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