法医学杂志

法医学杂志 ›› 2020, Vol. 36 ›› Issue (1): 41-44，51.DOI: 10.12116/j.issn.1004-5619.2020.01.009

• 论著 • 上一篇    下一篇

GC-MS衍生化方法快速检测生物样品中的氨

袁慧雅， 刘俊亭， 徐恩宇， 高利娜   

  1. 中国医科大学法医学院，辽宁 沈阳 110122
  • 发布日期:2020-02-25 出版日期:2020-02-28
  • 通讯作者: 刘俊亭，男，教授，博士研究生导师，主要从事体内药物和毒物分析研究；E-mail：liujunting8@163.com
  • 作者简介:袁慧雅（1988—），女，硕士，讲师，主要从事体内药物和毒物分析研究；E-mail：hyyuan@cmu.edu.cn
  • 基金资助:
    国家自然科学基金资助项目（81671864，81601644）

Rapid Determination of Ammonia in Biological Samples by GC-MS Derivatization Method

YUAN Hui-ya, LIU Jun-ting, XU En-yu, GAO Li-na   

  1. School of Forensic Medicine, China Medical University, Shenyang 110122, China
  • Online:2020-02-25 Published:2020-02-28

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摘要： 目的 建立生物样品中氨的气质联用定性和定量检测方法。 方法 采用七氟丁酰氯衍生化，气相色谱-质谱联用仪（gas chromatography-mass spectrometry，GC-MS）检测。考察不同pH值条件、衍生化温度、时间和不同提取溶剂对检测结果的影响，优化前处理条件。 结果 该方法能够准确检测血浆中氨的含量，检出限为0.1 μg/mL，目标物在0.5~200.0 μg/mL范围内线性关系良好（R2=0.987 7），日内精密度相对标准偏差范围为2.59%~3.88%，日间精密度相对标准偏差范围是3.21%~3.76%。 结论 该方法具有良好的灵敏度、稳定性和专属性，可用于法医毒物分析与临床生化检测。

关键词: 法医毒理学, 气相色谱-质谱法, 氨, 血浆, 衍生化

Abstract: Objective To establish a qualitative and quantitative method to determine ammonia in biological samples by gas chromatography-mass spectrometry （GC-MS）. Methods A heptafluorobutyryl chloride derivatization method was used. GC-MS was used for determination. The effects of different pH conditions, derivatization temperature, time and different extraction solvents on the test results were investigated. The pretreatment conditions were optimized. Results This method could accurately detect the ammonia content in blood, and the limit of detection was determined to be 0.1 μg/mL. The target component showed good linearity in the range of 0.5-200.0 μg/mL （R2=0.987 7）. The relative standard deviation range of intra-day precision was 2.59%-3.88%. The relative standard deviation range of inter-day precision was 3.21%-3.76%. Conclusion The method showed good sensitivity, stability and specificity, therefore can be used for forensic toxicology analysis and clinical biochemical detection.

Key words: forensic toxicology, gas chromatography-mass spectrometry, ammonia, plasma, derivatization