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Determination of Morphine and Codeine in Human Urine by Gas Chromatography-Mass Spectrometry

机译:气相色谱-质谱法测定人尿中的吗啡和可待因

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摘要

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 μm) 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.
机译:建立了灵敏,选择性的气相色谱-质谱(GC-MS)方法,并验证了该方法可用于测定人尿中的吗啡和可待因。建立了GC-MS条件。在具有温度程序的HP-1MS色谱柱(30μm×0.25μm,0.25μm)上进行分析,并使用氦气作为载气,流速为1.0μmL/ min。选定的离子监测(SIM)模式用于定量吗啡和可待因。优化了衍生溶剂,温度和时间。最后将丙酸酐和吡啶的混合溶剂(5 :: 2)用于80°C的衍生反应3min。在浓度范围为25-2000.0ng / mL时获得线性校准曲线,定量下限为25μng/ mL。日内和日间精度(RSD)值均低于13%,精度范围为87.2–108.5%。该方法已成功用于人尿中吗啡和可待因的测定,以进行法医鉴定研究。

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