【摘要】 目的探讨气相色谱-质谱联用法在检测人体血液、尿液中四氢大麻酚(THC)、四氢大麻酚酸(THC-COOH)、大麻酚(CBN)、大麻二酚(CBD)的含量的应用价值。方法人体样本(血、尿)经水解后制成弱酸性水液,加入含氘代四氢大麻酚(THC-D3)和含氘代四氢大麻酚酸(THC-COOH-D3)试剂作为内标,固相萃取(SPE)方法提取生物样本中的四氢大麻酚(THC)、四氢大麻酚酸(THC-COOH)、大麻酚(CBN)、大麻二酚(CBD),与硅烷化试剂BSTFA(含1%TMCS)进行衍生化后,采用气相色谱-质谱联用方法进行含量测定。结果血样:四氢大麻酚(THC)、大麻酚(CBN)、大麻二酚(CBD)、四氢大麻酚酸(THC-COOH)分别在10~80ng/mL的范围内与峰面积呈良好的线性关系,相关系数(R2)>0.996 7,平均回收率为91.8%~97%,相对标准误差(RSD)为0.59%~1.8%。5例血样THC含量分别为12、19、13、30、23ng/mL。3例血样CBN含量分别为43、47、56ng/mL,2例血样CBN含量<40ng/mL。2例血样CBD含量分别为55、60ng/mL,3例血样CBD含量<50ng/mL。4例血样THC-COOH含量分别为47、50、61、86ng/mL,1例血样THC-COOH含量<10ng/mL。尿样:四氢大麻酚(THC)、大麻酚(CBN)、大麻二酚(CBD)、四氢大麻酚酸(THC-COOH)分别在50~400ng/mL的范围内与峰面积呈良好的线性关系,相关系数(R2)>0.997 4,平均回收率为93.1%~99.3%,相对标准误差(RSD)为0.27%~1.16%,5例尿样中由于大部分THC酸化形成THC-COOH,因此没有THC或者浓度达不到最低检出限。1例尿样CBN含量为41ng/mL,1例尿样CBN含量<40ng/mL,3例尿样CBN含量<10ng/mL。3例尿样CBD含量分别为71、56、50ng/mL,1例尿样CBD含量<50ng/mL,1例尿样CBD含量<15ng/mL。5例尿样THC-COOH含量分别为88.4、99、53、47、65ng/mL。结论该方法简便、准确,可同时检测四氢大麻酚(THC)、四氢大麻酚酸(THC-COOH)、大麻酚(CBN)、大麻二酚(CBD)的含量。更多还原

【Abstract】 Objective To investigate GC-MS methods value in the detection of contents of tetrahydrocannabinol(THC),THC acetic acid(THC-COOH),cannabinol(CBN)and cannabidiol(CBD)in human samples(blood,urine).Methods Hydrolized human urine and blood samples were made as solution of weak acid,adding deuterated THC(THC-D3)and deuterated THCA(THC-COOH-D3)as an internal standard reagent,using solid phase extraction(SPE)to extract THC,THC-COOH,CBN and CBD from the samples,after silylating agent BSTFA(containing 1% TMCS)derivatizing to determine the contents by GCMS method.Results In the blood samples,the contents of THC,THC-COOH,CBN and CBD had good linear relationship with their peak areas within 10-80μg/L,in which correlation coefficient R2 was>0.9967,the average recovery rate was 91.8%-97% and the relative standard deviation(RSD)was0.59%-1.8%.The contents of THC in 5cases of blood sample were 12,19,13,30,23μg/L respectively,the contents of CBN in 3cases of blood were 43,47,56μg/L respectively,the contents of CBN in 2 cases of blood were<40μg/L,the contents of CBD in 2 cases of blood were 55,60μg/L,the contents of CBD in 3cases of blood were<50μg/L,the contents of THC-COOH in 4 cases of blood sample were 47,50,61,86μg/L respectively,and the contents of THC-COOH in 1 cases of blood sample was<25μg/L.In the urine samples,the contents of THC,THC-COOH,CBN and CBD had good linear relationship with their peak areas within 50-400μg/L,in which correlation coefficient R2 was>0.9974,the average recovery rate was 93.1%-99.3% and the relative standard deviation(RSD)was 0.27%-1.16%.Since most of the THC was acidized to THC-COOH,there was no THC or less than the limit of detection of THC in 5 cases of urine sample.The content of CBN in 1 cases of urine was 41μg/L,the content of CBN in 1 cases of urine was<40μg/L,the contents of CBN in 3cases of urine were<20μg/L,the contents of CBD in 3 cases of urine were 71,56,50μg/L respectively,the content of CBD in 1cases of urine was<50μg/L,the content of CBD in 1 cases of urine was<15μg/L,and the contents of THC-COOH in 5 cases of urine were 88.4,99,53,47,65μg/L respectively.Conclusion The method is simple and accurate,which could simultaneously detect the contents of THC,THC-COOH,CBN and CBD.更多还原