食品科学 ›› 2020, Vol. 41 ›› Issue (4): 262-267.doi: 10.7506/spkx1002-6630-20190326-335

• 安全检测 • 上一篇    下一篇

同位素内标-气相色谱-质谱法同时测定婴幼儿配方粉中3-氯丙醇酯和缩水甘油酯的含量

王亚,高红波,隋海霞,仇凯,钟其顶,吕晓玲   

  1. (1.天津科技大学食品科学与工程学院,天津 300457;2.中国食品发酵工业研究院,北京 100015;3.全国食品发酵标准化中心,北京 100015;4.国家食品安全风险评估中心,北京 100022)
  • 出版日期:2020-02-25 发布日期:2020-03-02
  • 基金资助:
    “十三五”国家重点研发计划重点专项(2016YFF0203903;2018YFC1603203); 中国食品科学技术学会食品科技基金——雅培食品营养与安全专项科研基金项目(2017-17)

Simultaneous Determination of 3-Monochloropropane-1,2-Diol Esters and Glycidyl Esters in Infant Formula Powder by Isotope Internal Standard-Gas Chromatography-Mass Spectrometry

WANG Ya, GAO Hongbo, SUI Haixia, QIU Kai, ZHONG Qiding, Lü Xiaoling   

  1. (1. College of Food Science and Engineering, Tianjin University of Science & Technology, Tianjin 300457, China;2. China National Research Institute of Food & Fermentation Industries, Beijing 100015, China;3. China National Standardization Center of Food & Fermentation, Beijing 100015, China;4. China National Center for Safety Risk Assessment, Beijing 100022, China)
  • Online:2020-02-25 Published:2020-03-02

摘要: 建立同时测定婴幼儿配方粉中3-氯丙醇酯和缩水甘油酯含量的方法,并检测我国市售部分婴幼儿配方粉中3-氯丙醇酯和缩水甘油酯的含量。结果表明,在最优条件下,3-氯丙醇酯和缩水甘油酯在0.050~0.80 mg/L范围内呈现良好的线性关系,R2均大于0.998,3-氯丙醇酯的加标回收率在81.4%~86.2%,相对标准偏差为4.42%~4.84%,缩水甘油酯的加标回收率为94.5%~101.1%,相对标准偏差为4.46%~6.12%,方法的检出限均为30 μg/kg。方法灵敏度高,精密度良好,适用于婴幼儿配方粉中3-氯丙醇酯和缩水甘油酯的定量检测。30 份市售婴幼儿配方粉样品中3-氯丙醇酯的含量为50.0~207.8 μg/kg,平均值为98.0 μg/kg,缩水甘油酯的含量为50.0~480.0 μg/kg,平均值为208.1 μg/kg。

关键词: 同位素内标-气相色谱-质谱法, 3-氯丙醇酯, 缩水甘油酯, 婴幼儿配方粉, 定量测定

Abstract: The aim of this study was the development of a method for the simultaneous determination of 3-monochloropropane-1,2-diol esters (3-MCPDEs) and glycidyl esters (GEs) in infant formula milk powder. Commercial infant formulas available on the Chinese market (n = 30) were analyzed for 3-MCPDEs and GEs by gas chromatography-mass spectrometry (GC-MS). Under the optimized conditions, 3-MCPDEs and GEs showed good linearity in the concentration range of 0.050?0.80 mg/L with correlation coefficient (R2) larger than 0.998. The mean recoveries from spiked samples were in the range of 81.4%?86.2% and 94.5%?101.1% with relative standard deviations (RSDs) ranging from 4.42% to 4.84% and from 4.46% to 6.12% for 3-MCPDEs and GEs, respectively. The limit of detection (LOD) of the proposed method was 30 μg/kg for both 3-MCPDEs and GEs. This method showed the advantages of high sensitivity, and accuracy, and could be suitable for the simultaneous detection of 3-MCPDEs and GEs in infant formula milk powder. In the 30 infant formula samples, levels of 3-MCPDEs and GEs ranged from 50.0 to 207.8 μg/kg and from 50.0 to 480.0 μg/kg with an average of 98.0 and 208.1 μg/kg, respectively.

Key words: isotope internal standard-gas chromatography-mass spectrometry, 3-monochloropropane-1,2-diol esters, glycidol esters, infant formula powder, quantitative determination

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