Yuan H Y, Liu J T, Xu E Y, Gao L N
School of Forensic Medicine, China Medical University, Shenyang 110122, China.
Fa Yi Xue Za Zhi. 2020 Feb;36(1):41-44. doi: 10.12116/j.issn.1004-5619.2020.01.009.
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 （=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.
目的 建立气相色谱 - 质谱联用（GC - MS）法测定生物样品中氨的定性及定量方法。方法 采用七氟丁酰氯衍生化法，利用GC - MS进行测定，考察不同pH条件、衍生化温度、时间及不同提取溶剂对检测结果的影响，优化预处理条件。结果 该方法能准确检测血液中的氨含量，测定检出限为0.1μg/mL。目标成分在0.5 - 200.0μg/mL范围内线性良好（r = 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为3.21% - 3.76%。结论 该方法具有良好的灵敏度、稳定性和特异性，可用于法医毒理学分析及临床生化检测。
