色谱 ›› 2019, Vol. 37 ›› Issue (2): 227-232.DOI: 10.3724/SP.J.1123.2018.09024

• 研究论文 • 上一篇    下一篇

气相色谱测定食品中丙酸及其盐类

李霞1, 刘旭2, 李玲1, 王艳丽1, 田其燕1, 刘艳明1   

  1. 1. 山东省食品药品检验研究院, 山东 济南 250000;
    2. 山东省环境执法局, 山东 济南 250000
  • 收稿日期:2019-09-17 出版日期:2019-02-09 发布日期:2014-12-31
  • 通讯作者: 刘艳明,Tel:(0531)81216719,E-mail:msymliu@163.com
  • 基金资助:

    国家重点研发计划项目(2017YFC1601600).

Determination of propionic acid and its salts in food by gas chromatography

LI Xia1, LIU Xu2, LI Ling1, WANG Yanli1, TIAN Qiyan1, LIU Yanming1   

  1. 1. Shandong Institute for Food and Drug, Jinan 250000, China;
    2. Shandong Environmental Law Enforcement Agency, Jinan 250000, China
  • Received:2019-09-17 Online:2019-02-09 Published:2014-12-31
  • Supported by:

    National Key Research and Development Program of China (No. 2017YFC1601600).

摘要:

建立了气相色谱测定食品中丙酸及丙酸盐的分析方法。针对含油脂和不含油脂的食品,分别建立了脱脂提取法和直接提取法。考察不同pH值对丙酸溶解性和加标回收率的影响,通过对净化条件、pH值、提取剂的种类和提取次数等条件的优化,确定最佳处理条件为:样品加盐酸溶液调节pH ≤ 2,用5 mL正己烷脱脂,用5 mL乙酸乙酯提取2次,合并提取液,使用HP-INNOWAX毛细管色谱柱对丙酸进行分离,用氢火焰离子化检测器检测,外标法定量。结果表明,使用脱脂提取法得到丙酸的回收率为87.5%~97.6%,相对标准偏差为3.09%~6.86%(n=6);使用直接提取法得到丙酸的平均回收率为90.1%~102.1%,相对标准偏差为3.32%~6.33%(n=6)。两种方法的线性范围为2~1000 mg/L(相关系数为0.9998),检出限为0.003 g/kg,定量限为0.01 g/kg。方法适用于多种食品中丙酸的检测,具有准确、快速、简便、灵敏度高等优点,为食品中丙酸含量的测定提供了新途径。

关键词: pH, 丙酸, 气相色谱, 食品, 脱脂提取法, 直接提取法

Abstract:

A method for the determination of propionic acid and its salts in food by gas chromatography (GC) was developed. Degrease extraction and direct extraction were established for food containing oil and non-oil, respectively. In this study, the effects of different pH values on the solubility and recovery of propionic acid were investigated. The effects of purification conditions, pH values, extraction agent types, and extraction times were studied. After hydrochloric acid solution was added, the pH levels of sample solutions were all found to be less than 2. The sample solutions were degreased with 5 mL n-hexane and extracted twice with 5 mL ethyl acetate. The analytes were detected by GC. The analytes were separated on an HP-INNOWAX chromatographic column and detected by fame ionization detector (FID). The recoveries of degrease extraction were 87.5%-97.6% and relative standard deviation were 3.09%-6.86% (n=6). The recoveries of direct extraction were 90.1%-102.1% and the relative standard deviations were 3.32%-6.33% (n=6). The two methods showed good linearities in the range of 2-1000 mg/L (correlation coefficient is 0.9998). The limit of detection was 0.003 g/kg and the limit of quantification was 0.01 g/kg. The proposed method is accurate, fast, simple, easy, sensitive, and is suitable for the rapid determination of propionic acid and its salts in different food. The proposed method provides a new way for the determination of propionic acid in food.

Key words: degrease extraction, direct extraction, food, gas chromatography (GC), pH, propionic acid

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