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气相色谱-质谱法测定人尿中吗啡和可待因。

Determination of morphine and codeine in human urine by gas chromatography-mass spectrometry.

机构信息

School of Pharmacy of Wenzhou Medical University, Wenzhou 325035, China.

出版信息

J Anal Methods Chem. 2013;2013:151934. doi: 10.1155/2013/151934. Epub 2013 Oct 10.

Abstract

A sensitive and selective gas chromatography-mass spectrometry (GC-MS) method was developed and validated for the determination of morphine and codeine in human urine. The GC-MS conditions were developed. The analysis was carried out on a HP-1MS column (30 m × 0.25 mm, 0.25  μ m) with temperature programming, and Helium was used as the carrier gas with a flow rate of 1.0 mL/min. Selected ion monitoring (SIM) mode was used to quantify morphine and codeine. The derivation solvent, temperature, and time were optimized. A mixed solvent of propionic anhydride and pyridine (5 : 2) was finally used for the derivation at 80°C for 3 min. Linear calibration curves were obtained in the concentration range of 25-2000.0 ng/mL, with a lower limit of quantification of 25 ng/mL. The intra- and interday precision (RSD) values were below 13%, and the accuracy was in the range 87.2-108.5%. This developed method was successfully used for the determination of morphine and codeine in human urine for forensic identification study.

摘要

建立并验证了一种灵敏、专属性的气相色谱-质谱联用(GC-MS)法,用于检测人尿液中的吗啡和可待因。优化了 GC-MS 条件。分析在 HP-1MS 柱(30m×0.25mm,0.25μm)上进行,采用程序升温,载气为氦气,流速为 1.0mL/min。采用选择离子监测(SIM)模式对吗啡和可待因进行定量分析。对衍生溶剂、温度和时间进行了优化。最终采用丙酸酐和吡啶(5:2)的混合溶剂在 80°C 下衍生 3min。在 25-2000.0ng/mL 浓度范围内得到线性校准曲线,定量下限为 25ng/mL。日内和日间精密度(RSD)值均低于 13%,准确度在 87.2-108.5%范围内。该方法成功用于法医鉴定研究中检测人尿液中的吗啡和可待因。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8705/3810378/bc3a670ca9a7/JAMC2013-151934.001.jpg

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