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目的建立尿液中四氢大麻酚(THC)、四氢大麻酸(THCA)的气相色谱串联质谱测定方法。方法尿样加入四氢大麻酸-D3(Δ9-THCA-D3)为内标,100℃水浴中氢氧化钾水解20 min、调pH,正庚烷振荡提取10 min,上层有机相吹干后经双(三甲基硅基)三氟乙酰胺(BSTFA)硅烷化70℃加热40 min衍生,利用气相色谱-串联质谱多反应监测(MRM)模式测定,内标法定量。结果本法平均加标回收率为90%~110%,相对标准偏差(RSD)为3.4%~6.3%,在0.25μg/ml~5μg/ml范围内具有良好的线性关系,线性相关系数(r)为:THC:0.9992,THCA:0.9998,最低检出浓度:THC:0.01μg/ml,THCA:0.05μg/ml。结论本法灵敏度高、准确性好,具有可靠的精密度与准确度,可用于尿样中四氢大麻酚、四氢大麻酸的同时测定。
Objective To establish a method for the determination of tetrahydrocannabinol (THC) and tetrahydrocannabinol (THCA) in urine by gas chromatography tandem mass spectrometry. Methods The urine sample was treated with tetrahydrocannabinol-D3 (Δ9-THCA-D3) as internal standard and hydrolyzed by potassium hydroxide in water bath at 100 ℃ for 20 min. The pH value was adjusted with n-heptane and extracted for 10 min. The upper organic phase was dried Derivatization of bis (trimethylsilyl) trifluoroacetamide (BSTFA) silanized with heating at 70 ℃ for 40 min was determined by gas chromatography-tandem mass spectrometry (MRM) mode and quantified by internal standard method. Results The average recoveries were 90% ~ 110% and the relative standard deviations (RSDs) ranged from 3.4% to 6.3%. The linear regression coefficients (r) ranged from 0.25μg / ml to 5μg / ): THC: 0.9992, THCA: 0.9998, the lowest detected concentration: THC: 0.01 μg / ml, THCA: 0.05 μg / ml. Conclusion This method has high sensitivity, good accuracy and reliable precision and accuracy. It can be used for simultaneous determination of tetrahydrocannabinol and tetrahydrocannabinol in urine samples.