柱切换LC-MS/MS分析吸毒尿样中的吗啡、O6-单乙酰吗啡、可待因、乙酰可待因

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×25 μm，分析柱为Xterra MS C₁₈ 2.1 mm×150 mm×3.5 μm，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。100 μL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 0.3～1 μg/L，线性关系良好，相关系数γ在0.999 1以上。

Determination of Morphine, O6-Monoacetyimorphine, Codeine and Acetylcodeine in Heroin Addicts' Urine by On-Line Solid-Phase Extraction (Column Switching) Liquid Chromatography with Tandem Mass Spectrometry

Morphine， O6 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.