SPE-GC-FID法测定婴幼儿配方奶粉中饱和烃类矿物油
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(湖南省产商品质量检验研究院,湖南 长沙 410017)

作者简介:

唐万里,男,湖南省产商品质量检验研究院工程师,硕士。

通讯作者:

冯燕英(1993—),女,湖南省产商品质量检验研究院助理工程师,硕士。E-mail:307351506@qq.com

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湖南省市场监督管理局科技计划项目(编号:2021KJJH49,2022KJJH55)


Solid phase extraction-gas chromatography-flame ionization detection (SPE-GC-FID) for the detection of mineral oil saturated hydrocarbons (MOSH) in infant formula
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(Hunan Provincial Institute of Product and Goods Quality Inspection, Changsha, Hunan 410017, China)

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    摘要:

    目的:建立可准确测定婴幼儿配方奶粉中饱和烃类矿物油(MOSH)的固相萃取结合气相色谱—氢火焰离子化检测器(SPE-GC-FID)分析方法。方法:以MOSH的提取量为考察指标,研究了不同提取方法(浸泡提取、振荡提取、超声辅助提取及液液萃取等)和提取溶剂(正己烷、异辛烷、苯及混合溶剂等)对婴幼儿配方奶粉中MOSH的提取效果,确定了最佳提取方法和提取溶剂。在此基础上,利用AgNO3 SPE固相萃取柱净化提取液,并用气相色谱—氢火焰离子化检测器(GC-FID)进行分析测定。结果:MOSH在10.0~1 000 μg/mL范围内具有良好线性关系,相关系数R2=0.999 97。方法的检出限为1.0 mg/kg,定量限为3.0 mg/kg。MOSH的加标回收率为93.3%~103.7%,相对标准偏差为2.3%~5.9%。应用该方法检测市售8个婴幼儿配方奶粉中的MOSH含量,结果在1.06~9.83 mg/kg,表明婴幼儿配方奶粉存在一定的MOSH污染风险。结论:该方法准确、灵敏,适用于婴幼儿配方奶粉中MOSH的检测。

    Abstract:

    Objective: To establish a new accurate method for the determination of mineral oil saturated hydrocarbon (MOSH) in infant formula by solid phase extraction combined with gas chromatography-Flame Ionization Detection (SPE-GC-FID). Methods: Different extraction methods such as soaking extraction, oscillating extraction, ultrasonic assisted extraction, liquid-liquid extraction were used to extract MOSH from infant formula milk powder, and different extraction solvents such as n-hexane, isooctane, benzene, mixed solvents were used to extract MOSH. The optimal extraction method and extraction solvent were determined based on the extraction amount of MOSH. The target compounds purified by AgNO3 SPE column, and finally detected by gas chromatography-Flame Ionization Detection (GC-FID). Results: The calibration curve of MOSH was linear in the range of 10.0~1 000 μg/mL with correlation coefficient of 0.999 97. The limit of detection was 1.0 mg/kg, and the limit of quantitation was 3.0 mg/kg. The recoveries from spiked samples were 93.3%~103.7%, and the relative standard deviations were 2.3%~5.9%. The MOSH in 8 commercially available infant formula was detected by the established method, and the results were between 1.06 and 9.83 mg/kg, indicating that there was a certain risk of MOSH contamination in infant formula. Conclusion: This method is accurate, sensitive, and suitable for the detection of MOSH in infant formula.

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唐万里,冯燕英,向 俊,等. SPE-GC-FID法测定婴幼儿配方奶粉中饱和烃类矿物油[J].食品与机械,2023,39(10):69-74.
TANG Wanli, FENG Yanying, XIANG Jun, et al. Solid phase extraction-gas chromatography-flame ionization detection (SPE-GC-FID) for the detection of mineral oil saturated hydrocarbons (MOSH) in infant formula[J]. Food & Machinery,2023,39(10):69-74.

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  • 收稿日期:2023-06-23
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  • 在线发布日期: 2023-12-26
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