食品科学 ›› 2017, Vol. 38 ›› Issue (6): 315-320.doi: 10.7506/spkx1002-6630-201706049

• 安全检测 • 上一篇    

超高效液相色谱-串联质谱法测定猪肉中β-受体激动剂残留量的不确定度分析

宁 霄,金绍明,梁瑞强,曹 进,张庆生   

  1. 中国食品药品检定研究院,北京 100050
  • 收稿日期:2017-03-30 修回日期:2017-03-30 出版日期:2017-03-25 发布日期:2017-03-28

Uncertainty Evaluation for the Determination of β-Agonists in Pork by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

VNING Xiao, JIN Shaoming, LIANG Ruiqiang, CAO Jin, ZHANG Qingsheng   

  1. National Institutes for Food and Drug Control, Beijing 100050, China
  • Received:2017-03-30 Revised:2017-03-30 Online:2017-03-25 Published:2017-03-28

摘要: 采用超高效液相色谱-串联质谱法对猪肉中沙丁胺醇、盐酸克伦特罗和莱克多巴胺含量的不确定度进行评估。根据JJF 1135—2005《化学分析测量不确定度评定》和JJF 1059.1—2012《测量不确定度评定与表示》中的有关规定,建立测定猪肉中3 种β-受体激动剂残留量不确定度的数学模型,逐层对不确定度来源进行分析。通过对不确定度分量进行量化和合成,得出当猪肉中沙丁胺醇含量为1.99 μg/kg时,其扩展不确定度为0.25 μg/kg(k=2);当猪肉中盐酸克伦特罗含量为2.04 μg/kg时,其扩展不确定度为0.24 μg/kg(k=2);当猪肉中莱克多巴胺含量为1.97 μg/kg时,其扩展不确定度为0.24 μg/kg(k=2)。评定结果表明,影响检测结果的主要因素为标准溶液配制、标准曲线拟合和测量重复性等。

关键词: 超高效液相色谱-串联质谱, 沙丁胺醇, 盐酸克伦特罗, 莱克多巴胺, 不确定度, 猪肉

Abstract: This study aimed to evaluate the uncertainty of measurement in the determination of salbutamol, clenbuterol hydrochloride and ractompaine in pork by ultra performance liquid chromatography-tandem mass spectrometry (UPLCMS/ MS). According to JJF 1135-2005 Evaluation of Uncertainty in Chemical Analysis Measurement and JJF 1059.1-2012 Evaluation and Expression of Uncertainty in Measurement, a mathematical model was established for uncertainty evaluation. The sources of uncertainty that may be introduced were analyzed and each component of uncertainty was quantified for the calculation of the combined uncertainty. The results showed that an expanded uncertainty of 0.25 μg/kg (k = 2) was obtained for the determination of the presence of 1.99 μg/kg salbutamol in pork, the expanded uncertainty was 0.24 μg/kg (k = 2) for the determination of pork samples containing 2.04 and 1.97 μg/kg salbutamol. The preparation of standard solution, curve fitting and measurement repeatability were found to be the main sources of uncertainty.

Key words: ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), salbutamol, clenbuterol hydrochloride, ractompaine, uncertainty, pork

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