应用气相色谱-质谱法结合统计方法对尿液中3种常见毒品分析结果的判定方法

Judgement of Analytical Results of 3 Common Drugs in Urine Given by GC-MS in Combination with Statistics

采集来自不同人群的尿液样品10份,并在此基础上加入杜冷丁、美沙酮和可卡因等3种毒品的混合标准溶液配制多份加标尿样,其中毒品的含量分别为其检出限的1,2倍,测定下限的1,1.5,2,4,6,8倍。这些样品分别按以下方法处理:取尿液样品1.0mL,加入100g·L^-1氢氧化钠溶液15μL,100mg·L^-1内标溶液20μL,加入环己烷1.0mL进行超声提取,离心后取上清液200μL,按仪器工作条件进行气相色谱-质谱法(GC-MS)测定。取空白尿液样品加入3种毒品的标准储备溶液,按上述方法绘制标准曲线,3种毒品的检出限(3S/N)依次为0.10,0.30,0.15mg·L^-1。用Spss软件对所测得的6千多个数据进行统计处理,获得3种毒品保留时间的绝对偏差在±0.04min(2.4s)内,相对保留时间的相对偏差在±0.1%内。特征离子离子比率的绝对偏差和相对偏差的判定范围分别为±20%内和±50%内。上述结果可为尿液中3种常见毒品分析结果的判定提供实际数据和理论依据。

Ten samples of human urine were collected from various multitudes,and a series of the urine samples were prepared by addition of mixed standard solutions of the 3 drugs,meperidine,methadone and cocaine to the 10 urine samples with their concentrations of 1 and 2 fold of the detection limits and 1,1.5,2,4,6,and 8 fold of the lower limits of determination.Each of these samples was pretreated as follows:1.0 mL of the urine sample was taken and added with 15μL of 100 g·L^-1 NaOH solution and 20μL of the internal standard solution of100 mg·L^-1.Then the solution was ultrasonically extracted with 1.0 mL of cyclohexane.After centrifugation,an aliquot of 200μL of the supernatant was taken for GC-MS determination according to the working conditions of the instruments.Standard curves were prepared by addition of standard stock solution of the 3 drugs to blank urine samples and treated as described above.Detection limits(3 S/N)of 0.10,0.30,0.15 mg·L^-1 were found for the 3 drugs respectively.About more than 6 000 data obtained in the analysis were treated statistically by using Spss software.The absolute deviations of retention time of the 3 drugs were found within ±0.04 min(2.4 s),and relative deviations of relative retention time of the 3 drugs were found to be within±0.1%.Determination ranges of absolute deviations and relative deviations of ionic ratios of characteristic ions were±20%and±50%,respectively.The results obtained were the practical data and theoratical basis for judgement of analytical results of the 3 common drugs in urine.