柱切换LC-MS/MS分析吸毒尿样中的吗啡、O^6-单乙酰吗啡、可待因、乙酰可待因

Determination of Morphine,O^6-Monoacetylmorphine,Codeine and Acetylcodeine in Heroin Addicts' Urine by On-Line Solid-Phase Extraction(Column Switching) Liquid Chromatography with Tandem Mass Spectrometry

建立在线固相萃取即柱切换LC-MS/MS方法,分析吸毒者尿样中的吗啡、O6-单乙酰吗啡、可待因、乙酰可待因。以吗啡-d3为内标,预处理柱为Oasis(HLB 2.1 mm×20 mm×25μm,分析柱为Xterra(MS C182.1 mm×150 mm×3.5μm,用水作预处理流动相,分析流动相用含甲酸铵和甲酸的水、乙腈梯度洗脱,质谱采用电喷雾离子源,正离子MRM扫描。100μL尿样直接进样分析,尿样中吗啡、O6-单乙酰吗啡、可待因、乙酰可待因的检测限为0.3~1μg/L,线性关系良好,相关系数γ在0.999 1以上。

Morphine,O6-monoacetylmorphine,codeine and acetylcodeine in heroin addicts＇ urine samples were analyzed by on-line solid-phase extraction（column switching） liquid chromatography-tandem mass spectrum（LC-MS/MS）.The urine samples were directly injected into a extraction column（Oasis HLB 2.1 mm×20 mm×25 μm）.After a washing step with the extraction mobile phase,the retained compounds were flushed into the analytical column（Xterra MS C18 2.1 mm×150 mm×3.5 μm） with the analytical mobile phase and morphine-d3 as internal standard.The positive electricspray ionization mode was applied,multiple reaction monitoring（MRM） mode was used to analyze target compounds.Identification was based on the compound＇s retention time and two pairs of precursor-to-product ion transitions.The limit of detections（LODs） are 1 μg/L for morphine、codeine、O6-monoacetylmorphine and 0.3 μg/L for acetylcodeine.The method has excellent linearity,and the linear correlation coefficient is greather than 0.999 1.The method shows high sensitivity and selectivity,which is suitable for analysis of morphine,O6-monoacetylmorphine,codeine and acetylcodeine in heroin addicts＇ urine samples.