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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

摘    要
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1.0 mL,加入100 g·L-1氢氧化钠溶液15 μL,100 mg·L-1内标溶液20 μL,加入环己烷1.0 mL进行超声提取,离心后取上清液200 μL,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0.10,0.30,0.15 mg·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±0.04 min(2.4 s)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。
标    签 气相色谱-质谱法   杜冷丁   美沙酮   可卡因   判定   GC-MS   meperidine   methadone   cocaine   judgement  
 
Abstract
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 15 μL of 100 g·L-1 NaOH solution and 20 μL of the internal standard solution of 100 mg·L-1. Then the solution was ultrasonically extracted with 1.0 mL of cyclohexane. After centrifugation, an aliquot of 200 μL 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 (3S/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.

中图分类号 O657.63   DOI 10.11973/lhjy-hx201911003

 
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所属栏目 试验与研究

基金项目 公安部科技强警基础工作专项资助项目(2017GABJC06)

收稿日期 2019/3/20

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备注彭山珊,硕士研究生,主要从事毒物毒品分析研究工作

引用该论文: PENG Shanshan,XIN Guobin,WANG Jifen,WANG Yi,WANG Yanyan,MENG Jinjie. Judgement of Analytical Results of 3 Common Drugs in Urine Given by GC-MS in Combination with Statistics[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2019, 55(11): 1254~1260
彭山珊,辛国斌,王继芬,王伊,王燕燕,孟晋杰. 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[J]. 理化检验-化学分册, 2019, 55(11): 1254~1260


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参考文献
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【2】SANCO/12571/2013 Guidance document on analytical quality control and validation procedures for pesticide residues analysis in food and feed[S].
 
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