分散液液微萃取预处理-气相色谱-质谱法快速测定人尿中3种毒品方法改进  

Modification of Method for Rapid Determination of 3 Illicit Drugs in Human Urine by GC-MS with Pretreatment by DLLME

作　　者：刘缙 蔡红新 钱斌 董文彬[1] 毛海峰 梁晨[2] LIU Jin;CAI Hongxin;QIAN Bin;DONG Wenbin;MAO Haifeng;LIANG Chen(Institute of Criminal Science]inshan Branch of Shanghai Public Security Bureau,Shanghai 201508,China;Identic fication Center of Material Evi dense of Shanghai Public Security Bureau,Shanghai 200083,China)

机构地区：[1]上海市公安局金山分局刑事科学研究所,上海201508 [2]上海市公安局物证鉴定中心,上海200083

出　　处：《理化检验（化学分册）》2019年第12期1442-1447,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：对应用分散液液微萃取(DLLME)于气相色谱-质谱法(GC-MS)测定尿液中毒品的方法作了改进。分析时,在尿样2.0mL中加入20.0mg·L-1 SKF525A内标溶液100μL,并调节其酸度至pH 12后,增加了加入N-丙基乙二胺(PSA)50mg并振荡、离心的步骤,达到除去尿液中脂肪酸等杂质的目的,在后续操作中不会出现脂状沉淀。之后,取其上清液,加入分散剂异丙醇400μL和萃取剂四氯化碳20μL,轻轻振荡1min并离心5min后即可用微量移液器提取离心管尖底的小液滴1μL,按GC-MS工作条件测定尿样中甲基苯丙胺、3,4-亚甲基二氧基苯丙胺(MDMA)和氯胺酮等3种毒品,其标准曲线的线性范围均在0.1~10.0mg·L-1之间,检出限(3S/N)也相同,均为0.01mg·L-1。试验测得3者的平均回收率依次为76.4%,83.2%,103%;三者测定值的相对标准偏差(n=5)依次为6.7%,5.3%,6.7%(日内)和7.5%,5.9%,6.6%(日间)。A modification for the dispersion liquid-liquid micro extraction(DLLME)in the sample pretreatment of rapid determination of 3 illicit drugs(i.e.,methamphetamine,MDMA and ketamine)in human urine by GC-MS in hyphenation was proposed.In the analytical procedure,after the urine sample(2.0 mL)was mixed with 100μL of 20.0 mg·L-1 internal standard solution of SKF525 A,and its acidity was adjusted to pH 12,a modification of addition of 50 mg of PSA to the solution was made at this stage to remove impurities of fatty acid in urine,thus no precipitation of footy substance would happen in succeeding manipulations.After the addition of PSA,the mixture was centrifuged and the surpernatant was taken,to which 400μL of iso-propyl alcohol(as dispersant)and 200μL of CCl4(as extractant)were added.The mixture was shocked lightly for 1 min and centrifuged for 5 min.1μL of the extractant(CCl4)at the shape bottom of the centrifuging tube was taken with a micropipet,and used for GC-MS determination of the 3 illicit drugs.Standard curves of the 3 drugs were found to have the same linearity range between 0.1 to 10.0 mg·L-1 and same detection limit(3 S/N)of 0.01 mg·L-1.Test for recovery was made by standard addition method at 3 concentration levels,giving average recoveries of 76.4%,83.2%,103%for the 3 drugs respectively.Values of RSDs(n=5)found from the determined values of the 3 drugs were 6.7%,5.3%,6.7%(intraday)and 7.5%,5.9%,6.6%(interday)respectively.

关 键 词：气相色谱-质谱法 分散液液微萃取 毒品 刑侦毒物分析 

分 类 号：O657.31[理学—分析化学]