婴幼儿配方奶粉中氯丙醇脂肪酸酯的检测方法优化与污染暴露

doi:10.7506/spkx1002-6630-20180305-048

食品科学 ›› 2019, Vol. 40 ›› Issue (10): 311-317.doi: 10.7506/spkx1002-6630-20180305-048

婴幼儿配方奶粉中氯丙醇脂肪酸酯的检测方法优化与污染暴露

张妮，周静*，胡守江，叶青，彭亚锋，陆壹

上海市质量监督检验技术研究院，上海 200233

出版日期:2019-05-25 发布日期:2019-05-31
基金资助:
上海市科学技术委员会科研计划项目（16142201800）；上海市质量监督检验技术研究院科技项目（KY-2017-5-SP）；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）

Optimized Detection and Pollution Exposure of Chloropropanol Fatty Acid Esters in Infant Formula

ZHANG Ni, ZHOU Jing*, HU Shoujiang, YE Qing, PENG Yafeng, LU Yi

Shanghai Institute of Quality Inspection and Technical Research, Shanghai 200233, China

Online:2019-05-25 Published:2019-05-31

摘要/Abstract

摘要： 目的：采用气相色谱-质谱（gas chromatography-mass spectrometry，GC-MS）联用技术，建立同时测定婴幼儿配方奶粉中3-氯-1,2-丙二醇脂肪酸酯（3-monochloropropane-1,2-diol ester，3-MCPDE）、2-氯-l,3-丙二醇脂肪酸酯（2-monochloropropane-1,3-diol ester，2-MCPDE）、1,3-二氯-2-丙醇脂肪酸酯（1,3-dichloropropane-2-ol ester，1,3-DCPE）和2,3-二氯-1-丙醇脂肪酸酯（2,3-dichloropropane-1-ol ester，2,3-DCPE）含量的分析方法，并对市售50 份婴幼儿配方奶粉中4 种氯丙醇脂肪酸酯的污染水平进行调查分析和风险暴露评估。方法：婴幼儿配方奶粉经脂肪提取后，依次通过碱水解、硅藻土固相萃取小柱净化、七氟丁酰基咪唑衍生上机，同位素内标法定量。结果：该方法在20～600 ng/mL范围内线性良好（r2≥0.998 9），检出限为0.005 mg/kg，定量限为0.015 mg/kg，检出限和定量限均以相应的氯丙醇计。0.03、0.075 mg/kg和0.15 mg/kg水平下的加标回收率在82.2%～113.9%之间，相对标准偏差均不大于8.3%。50 份奶粉样品中，3-MCPDE检出率为100.0%，含量为0.037～0.208 mg/kg，2-MCPDE检出率为42.0%，含量为ND～0.060 mg/kg，1,3-DCPE和2,3-DCPE均未检出。统计不同月龄婴幼儿氯丙醇脂肪酸酯的平均暴露量，0～6 月龄为3.86 μg/kg、6～12 月龄为2.00 μg/kg、12～36 月龄为1.07 μg/kg。结论：该方法操作简便、准确可靠，适合婴幼儿配方奶粉中4 种氯丙醇脂肪酸酯的同时测定。婴幼儿摄入氯丙醇脂肪酸酯的健康风险需引起关注。

关键词: 氯丙醇脂肪酸酯, 气相色谱-质谱联用, 婴幼儿配方奶粉

Abstract: Objective: A method for the simultaneous determination of the contents of 3-monochloropropane-1,2-diol ester (3-MCPDE), 2-monochloropropane-1,3-diol ester (2-MCPDE), 1,3-dichloropropane-2-ol ester (1,3-DCPE) and 2,3-dichloropropane-1-ol ester (2,3-DCPE) in infant formula was established by gas chromatography-mass spectrometry (GC-MS). A total of 50 infant formula samples sold in Shanghai were researched for the pollution levels of four chloropropanol fatty acid esters (CPFAEs). Also we assessed the dietary exposure of infants to CPFAEs in infant formula. Methods: Fat was extracted from samples, followed by alkali hydrolysis, solid-phase extraction purification through a diatomite column and derivatization with heptafluoro butyrylimidazole before being injected into the GC-MS system. The analytes were quantified by the internal standard method. Results: The method showed a good linear relationship in the concentration range of 20–600 ng/mL (r2 ≥ 0.998 9). The limit of detection (LOD) and limit of quantification (LOQ) were 0.005 and 0.015 mg/kg, respectively (calculated as chlorpropanol). The recoveries of the four chloropropanols esters spiked at 0.03, 0.075 and 0.15 mg/kg were between 82.2%–113.9%, with relative standard deviations (RSDs) of less than 8.3%. 3-MCPDE and 2-MCPDE were detected in 100.0% and 42.0% of the 50 infant formula samples with contamination levels in the range of 0.037–0.208 mg/kg and ND–0.060 mg/kg, respectively. However, 1,3-DCPE and 2,3-DCPE were not detected in any sample. The average exposure to CPFAEs in infant formula were 3.86, 2.00 and 1.07 μg/kg for infants aged 0–6, 6–12 and 12–36 months, respectively. Conclusion: The method was easy to operate with good accuracy and reliability, and suitable for the determination of CPFAEs in infant formula. The health risk of CPFAEs through the intake of infant formula for infants should be a major concern.

Key words: chloropropanols fatty acid esters, gas chromatography-mass spectrometry (GC-MS), infant formula

中图分类号:

TS201.6

张妮，周静*，胡守江，叶青，彭亚锋，陆壹. 婴幼儿配方奶粉中氯丙醇脂肪酸酯的检测方法优化与污染暴露[J]. 食品科学, 2019, 40(10): 311-317.

ZHANG Ni, ZHOU Jing, HU Shoujiang, YE Qing, PENG Yafeng, LU Yi. Optimized Detection and Pollution Exposure of Chloropropanol Fatty Acid Esters in Infant Formula[J]. FOOD SCIENCE, 2019, 40(10): 311-317.

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婴幼儿配方奶粉中氯丙醇脂肪酸酯的检测方法优化与污染暴露

Optimized Detection and Pollution Exposure of Chloropropanol Fatty Acid Esters in Infant Formula

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