首页> 中文期刊>新疆医科大学学报 >GC、GC-MS 法定性定量法检测血液和尿液中阿片类毒品及其代谢物的含量

GC、GC-MS 法定性定量法检测血液和尿液中阿片类毒品及其代谢物的含量

     

摘要

Objective Establish gas chromatography (GC)and gas-mass spectrometry (GC-MS)methods to detect opioid drugs and their metabolites in the blood and urine.Methods Added pH6 phosphate buffer solution into urine or blood sample as 0.01 M to adjust pH at 5-6,brought it into solid phase extraction column (SPE),rinsed the column by deionized water and 0.01 M HCl,and then washed SPE column with CH3 OH.Extracted by CH2 Cl2/CH3 CH2 OHCH 3 mixture which were contained 2% ammonia and dried up,then derivatized with BSTFA+TMCS (99∶1)reagent,took SKF-525 as internal standard,tested the content of the sample by DB-5 MS chromatographic column at ion (m/z)scan mode (SIM)and the full scan model of GC and GC-MS.Results There were good linear relationship between the contents of drugs (heroin,morphine,codeine,6-acetyl codeine,6-acetyl morphine,and ethyl morphine)and peak area in the range of 25~400 μg/L,in which the correlation coefficient r was bigger than 0.9907;the average re-covery rate of internal standard was 95.9~ 101.6%;the relative standard error (RSD)was 2.13%;the minimum limit of detection (LOD)was 1 μg/L,the minimum limit of quantitative (LOQ)was 25 μg/L. Codeine,morphine and 6-acetyl morphine in case urine sample could be detected.The content of codeine was >400 μg/L,morphine was 384 μg/L,and 6-acetyl morphine was 278 μg/L,while detection amount of blood samples were extremely low,but the illegal facts of heroin could be confirmed.Conclusion The methods were simple,rapid,high sensitivity and accurate quantitative and qualitative,which will be suit-able for the screening and confirming test of blood and urine samples of drug addicters or drug abusers.%目的:建立检测血液、尿液中阿片类毒品及其代谢物含量的气相色谱(GC)法或气-质联用(GC-MS)法。方法尿样或血样中的阿片类毒品,加0.1 mol/mL (pH=6)磷酸缓冲溶液调节 pH 为5~6,将样品添加于固相萃取柱(SPE),用去离子水和0.1 mol/mL HCl 淋洗,再次用 CH3 OH 洗涤 SPE 柱子,由含2%氨水的 CH2 Cl2/CH3 CH2 OHCH3混合液萃取提取,吹干,用 BSTFA+TMCS(99∶1)试剂衍生化,以 SKF-525a 作为内标,利用色谱柱为 DB-5MS 的 GC、GC-MS 仪选择离子(m/z)扫描模式(SIM)和全扫描(Full Scan)模式进行测试分析。结果海洛因、吗啡、可待因、6-乙酰吗啡、6-乙酰可待因、乙基吗啡在25~400 ng/mL 范围内与峰面积呈良好的线性关系,相关系数 r >0.9907,平均加内标回收率为95.9%~101.6%,相对标准误差(RSD)为2.13%~8.59%,最低检测限(LOD)为1 ng/mL,最低定量限(LOQ)为25 ng/mL。案件样品尿液检测出可待因、吗啡成分、6-乙酰吗啡成分,可待因含量>400 ng/mL,吗啡为384 ng/mL,6-乙酰吗啡为278 ng/mL,血液检测量极小,确证了吸食海洛因的违法事实。结论本方法简单、快速、灵敏度高、准确定性定量,适用于吸毒或毒品滥用者血样、尿样的筛查与确认试验。

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