doi:10.16597/j.cnki.issn.1002-154x.2022.02.003

双柱双检测器顶空气相色谱法测定血液中乙醇含量的方法验证

赵顺新

(南京康宁司法鉴定中心,江苏 南京 210000)


Methord Verification of Determination of Alcohol in Blood Using Headspace Gas Chromatographic with Dual-column and Dual-detector Methord

Zhao Shunxin

(Nanjing Kangning Forensic Science Center. Jiangsu Nanjing 210000)


摘要:

目的:验证《血液酒精含量的检测方法》GA/ T 842—2019 在笔者所在实验室的适用性。 方法:本文利用顶空 进样器进样,叔丁醇作为内标,用装有两根色谱柱以及两个氢火焰离子化检测器的气相色谱仪进行分析,用保留时间 定性,内标标准曲线法定量。 同时测定了方法的检出限、定量限,精密度以及准确度。 结果:该方法线性范围为 5.0 ~ 300.0 mg / 100 mL,通道 A 线性回归方程为:Y = 0.010983X - 0.019970,R2 = 0.999967;通道 B 线性回归方程为:Y = 0.011 148x - 0.012 749,R2 = 0.999947, A 通道和 B 通道的检出限均为 1 mg/100 mL,定量限均为 5 mg/100 mL;两个通道进样的日间精密度和日内精密度的相对标准偏差 RSD 均小于 5.0% 。 A 通道的回收率在 99.32 ~ 101.40% 之间, B 通道的回收率在 99.40 ~ 100.20% 之间。 A 通道和 B 通道的扩展不确定度分别为 1.75 mg/100 mL 和 1.61 mg/100 mL。 结论:该实验室实验条件符合此方法的要求,能够满足血液中乙醇含量的检测工作。

关键词:双柱双检测器血液乙醇方法验证精密度

Abstract

Objective: Verify the adaptability of 《Examination methods for ethanol concentration in blood》GA/ T 842—2019 in author’s laboratory. Methods: The samples were analyzed by HS-GC that the tertiary butal alcohol was acted as the internal standard substance. The HS-GC was equipped with two chromatographic columns and two hydrogen flame ionization detector. The retention time of the peak was performed as qualitative parameter and the standard curves method of internal standard were acted as quantitative basis. At the same time, limit of detection and limit of quantification, precision and accuracy were determined. Results: The linearity of calibration was 5.0 ~ 300. 0 mg / 100 mL. Linear regression equation of channel A is Y = 0. 010 983X - 0. 019970 and R 2 = 0. 999967. Besides Linear regression equation of channel B is y = 0. 011 148x - 0. 012 749,R 2 = 0. 999 947. Detection limit of channel A and channel B were 1 mg / 100 mL. Quantification limit of channel A and channel B were 5 mg / 100 mL. Relative standard deviation (RSD) of channel A and channel B were less than 5% . Recovery rate of channel A was 99. 32 ~ 101. 40% . Besides, recovery rate of channel B was 99. 40 ~ 100. 20% . The expanded uncertainty of channel A and channel B were 1. 75 mg / 100 mL and 1. 61 mg / 100 mL respectively,when the concentration of ethanol in blood was 80 mg / 100 mL. Conclusion: The laboratory’s experimental conditions can comply with the requirements of the national standard. The laboratory can meet detection alcohol in blood.

Keywordsldual-column and dual-detector; blood; alcohol; method verification; precision;