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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。
Objective To investigate the content of THC, THC-COOH, CBN and CBD in human blood and urine by gas chromatography-mass spectrometry (GC-MS) Value. Methods Human samples (blood and urine) were hydrolyzed to make weak acid aqueous solution. THC-D3 and THC-COOH-D3 containing deuterated tetrahydrocannabinol (THC-COOH-D3) (THC), THC-COOH, CBN, CBD in biological samples were extracted by solid-phase extraction (SPE) After derivatization with BSTFA (containing 1% TMCS), the content was determined by gas chromatography-mass spectrometry. Results Blood samples showed good peak area with THC, CBN, CBD and THC-COOH in the range of 10 ~ 80ng / mL, respectively The correlation coefficient (R2) was 0.996 7, the average recovery was 91.8% -97%, and the relative standard deviation (RSD) was 0.59% -1.8%. 5 cases of blood THC content were 12,19,13,30,23ng / mL. The CBN contents of the three blood samples were 43, 47 and 56 ng / mL, respectively. The blood samples contained 2 CBN levels <40 ng / mL. Two cases of blood samples CBD content were 55,60ng / mL, three cases of blood samples CBD content <50ng / mL. The THC-COOH contents in 4 cases were 47, 50, 61 and 86 ng / mL, respectively, while the blood samples contained 1 THC-COOH <10 ng / mL. Urine samples showed good THC, CBN, CBD, and THC-COOH in the range of 50-400 ng / mL The relative standard deviation (RSD) was 0.27% ~ 1.16%. The majority of THC acidified THC-COOH in 5 urine samples, and the correlation coefficient was 0.997 4. The average recovery was 93.1% -99.3% So there is no THC or the concentration does not reach the minimum detection limit. One sample had a CBN content of 41 ng / mL, one CBN content of <40 ng / mL and three urine samples of CBN <10 ng / mL. The CBD contents of urine samples were 71, 56 and 50 ng / mL in 3 cases, CBD content in urine samples was less than 50 ng / mL in 1 case and CBD contents in 1 case were less than 15 ng / mL. The contents of THC-COOH in 5 cases were 88.4,99,53,47,65ng / mL, respectively. Conclusion The method is simple and accurate, and can simultaneously detect THC, THC-COOH, CBN and CBD.