论文部分内容阅读
本文报告阿片类药物依赖性患者尿标本中同时测定吗啡和可待因的气相色谱-质谱联用法(GC-MS)的方法学研究和部分病例尿标本的测定结果。尿标本(或含吗啡和可待因的尿标准溶液)加丙烯吗啡做为内标物,经酸性条件下水解后用有机溶剂提取纯化。提取物在无水吡啶中用醋酐进行乙酰化,乙酰化衍生物进样分析。定量方法采用选择离子检测法(SIM)。可待因、吗啡和内标物丙烯吗啡的保留时间分别为1.74,2.34和3.23min,选择三者的基峰341,327和353做为SIM定量的离子。可待因和吗啡的标准曲线线性范围分别为20-600μg/1和20-800μg/1。方法检测限为2μg/1,该浓度下两种药物的信/噪比为5:1。可待因和吗啡高,低浓度的精密度均良好,50和200μg/1可待因的日间变异系数(CV%)分别为3.12和1.64;相同浓度吗啡的日间变异分别为3.12和2.51。衍生化产物室温下48h内稳定。应用本法对阿片类药物依赖性患者近200份尿标本进行测定结果显示,该法可定量测得患者停用毒品后10d尿中的吗啡。
This paper reports the methodological study of simultaneous determination of morphine and codeine in urine samples by gas chromatography-mass spectrometry (GC-MS) and the determination of urinalysis in some cases of urine samples from opioid-dependent patients. Urinalysis (or urine standard solution containing morphine and codeine) plus propylene morphine as an internal standard was hydrolyzed with acid and purified with an organic solvent. The extract was acetylated with acetic anhydride in anhydrous pyridine and the acetylated derivative was injected for analysis. Quantitative methods using selective ion detection (SIM). The retention times of codeine, morphine and internal standard propylene morphine were 1.74, 2.34 and 3.23min, respectively. The base peaks 341, 327 and 353 of the three were selected as SIM quantitative ions. The standard curve for codeine and morphine has linear ranges of 20-600 μg / 1 and 20-800 μg / 1, respectively. The detection limit of the method was 2μg / 1, the signal / noise ratio of the two drugs at this concentration was 5: 1. The high and low concentrations of codeine and morphine were good, and the CV% of 50 and 200 μg / 1 codeine were 3.12 and 1.64 respectively. The daytime variability of the same concentration of morphine was 3.12 and 2.51. Derivatized products were stable within 48h at room temperature. The application of this method to opioid dependence in patients with nearly 200 urine samples were measured results show that the method can be measured quantitatively in patients with drug withdrawal 10d urinary morphine.