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目的建立快速、准确、灵敏的尿中四氢大麻酚(THC)和四氢大麻酸(THC-COOH)残留的分散固相萃取(d SPE)-高效液相色谱-串联质谱测定方法。方法尿液经酸化后,以PSA为分散固相萃取剂去除尿液中的杂质,经离心分离后,上清液经氮气吹干,残渣用流动相定容,试样在XBridge RP18色谱柱上,以乙腈-20 mmol/L乙酸铵溶液(70∶30,V/V)为流动相分离,电喷雾负离子模式下MRM法定量。结果 THC和THC-COOH标准溶液的浓度为0.5μg/L~50.0μg/L时,线性关系良好,其相关系数(r)均>0.999。尿液中THC和THC-COOH的LOD均为0.15μg/L,LOQ均为0.5μg/L。THC和THC-COOH的加标回收率为91.6%~98.9%,日内相对标准偏差(RSD)为2.1%~4.6%,日间RSD为4.4%~8.3%。结论本方法回收率高,净化效果显著,稳定性好,杂质干扰少,可用于吸毒者尿液中THC和THC-COOH的残留检测。
Objective To establish a rapid, accurate and sensitive method for the determination of residues of THC and THC-COOH in urine by d SPE-HPLC-tandem mass spectrometry. Methods After the urine was acidified, the PSA was used to disperse the solid phase extraction solvent to remove the impurities in the urine. After centrifugation, the supernatant was dried by nitrogen and the residue was fixed with a mobile phase. The sample was on a XBridge RP18 column , Separated by acetonitrile-20 mmol / L ammonium acetate solution (70:30, V / V) and quantified by MRM in negative ion electrospray ionization mode. Results When the concentration of THC and THC-COOH standard solution was 0.5μg / L ~ 50.0μg / L, the linearity was good and the correlation coefficient (r) was> 0.999. The LOD of urine and THC-COOH in urine were 0.15μg / L, LOQ was 0.5μg / L. The spiked recoveries of THC and THC-COOH ranged from 91.6% to 98.9%. The relative standard deviations (RSDs) ranged from 2.1% to 4.6%. The daytime RSD ranged from 4.4% to 8.3%. Conclusion The method has high recovery rate, significant purifying effect, good stability and less interference of impurities. It can be used for the residual detection of THC and THC-COOH in the urine of drug addicts.