固相萃取结合气相色谱质谱法检测牛奶中1,2-丙二醇
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1.山东药品食品职业学院食品系;2.江苏省疾病预防控制中心

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Determination of 1,2-propanediol in milk using the solid phase extraction combinedwith gas chromatography-mass spectrometry
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1.Department of Foods,Shandong Drug and Food Vocational College,Weihai;2.Jiangsu Center for Disease Prevention and Control,Nanjing

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    摘要:

    目的 建立了牛奶中1,2-丙二醇的固相萃取法富集净化,气相色谱-质谱法检测技术。方法 研究考察了牛奶检测中的前处理技术:蛋白沉淀技术,固相萃取技术,样品用亚铁氰化钾和醋酸锌沉淀蛋白,采用硅藻土固相萃取柱萃取净化。结果 在优化的条件下,在0.1~50 μg/mL范围内,1,2-丙二醇具有较好的线性相关性,线性相关系数为0.9994, 在0.33、0.5和2.0 mg/kg三个添加浓度,回收率、相对标准偏差分别为81.8~86.5%、3.1~5.8 %;方法的最低检出浓度为0.1 mg/kg。结论 方法操作简单,环保,灵敏度高,准确性好。

    Abstract:

    Objective Developed a method based on solid phase extraction(SPE) combined with gas chromatography-mass spectrometry (GC-MS) to determine 1,2-propanediol in milk. Methods The precipitation technology of protein and solid phase extraction,Pretreatment technology in milk testing,were carefully investigated. Protein of sample milk was precipitated by potassium ferrocyanide and zinc acetate, then cleaned-up by silicious earth solid phase extraction (SPE). Results In the range of 0.1 ~ 50 μg/mL,1,2-propanediol had good linear with R2 0.9994 under the selected conditions. The recovery and relative standard deviation(RSD) were 81.8~86.5 % and 3.1~5.8 % at 0.33、0.5 and 2.0 mg/kg spiked. And the minimum detection concentration of the method was 0.1 mg/kg. Conclusion The developed method has proved convenient, environmental- friendly, accurate and sensitive.

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  • 收稿日期:2024-05-31
  • 最后修改日期:2024-12-20
  • 录用日期:2025-01-12
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