UPLC和UPLC-MS/MS法检验工业大麻及其加工产品中Δ^(9)-四氢大麻酚

Δ^(9)-Tetrahydrocannabinol and other four components in industrial hemp and its processed products were detected by UPLC and UPLC-MS/MS methods

目的 对工业大麻植株花叶和大麻加工产品中的Δ^(9)-四氢大麻酚进行提取分离,建立Δ^(9)-THC的液相色谱-质谱(LC-MS)定性定量检验方法和液相色谱(LC)定量检验方法。方法 样品自然晾干后经过研磨,加入甲醇提取后进样分析,采用ACQUITY UPLC^(R)BEH C_(18)色谱柱,液相色谱以水、乙腈进行梯度洗脱,检测波长:215 nm,带宽:4.8nm。液相色谱-质谱以0.1%甲酸水、0.1%甲酸乙腈进行梯度洗脱,电喷雾离子源、扫描方式:正离子模式,多个特征离子对进行定性分析,外标标准曲线法进行定量分析。结果 工业大麻植株花叶和大麻加工产品在液相色谱中Δ^(9)-THC在0.001~0.1 mg/mL范围内线性良好,液相色谱-质谱中在5~100 ng/mL的范围内线性良好,R^(2)均> 0.999。液相色谱和液质联用检验方法的测量值相对误差均在±2%以内,精密度均<2%。结论 本文建立的方法可应用于工业大麻植株花叶和大麻加工产品中Δ^(9)-THC的检验,可为实验室针对工业大麻植株花叶和大麻加工产品中四氢大麻酚的检验提供技术支持。

Objective The Δ^(9)-tetrahydrocannabinol in the flowers and leaves of industrial hemp plants and hemp processing products was extracted and separated,to establish a liquid chromatography-mass spectrometry( LC-MS)qualitative and quantitative test method and a liquid chromatography( LC) quantitative test method for Δ^(9)-THC.Methods The samples were dried naturally and ground,extracted with methanol and analyzed.The ACQUITY UPLC^(R) BEH C_(18) column was used.The liquid chromatography was performed on a gradient elution with water and acetonitrile.The detection wavelength was 215 nm and the bandwidth was 4.8 nm.Liquid chromatography-mass spectrometry was performed with 0.1 % formic acid water and 0.1 % formic acid acetonitrile for gradient elution.Electrospray ion source,scanning mode:positive ion mode,multiple characteristic ion pairs for qualitative analysis,and externalstandard curve method for quantitative analysis.Results The linearity of Δ^(9)-THC in the range of 0.001 ~ 0.1 mg/mL in liquid chromatography and 5 ~ 100 ng/mL in liquid chromatography-mass spectrometry was good,R~2 were greater than 0.999.The relative error of the measured values of the liquid chromatography and liquid chromatography-mass spectrometry test methods was within ± 2 %,and the precision was less than 2 %.Conclusion The method established in this paper can be applied to the detection of Δ^(9)-THC in industrial cannabis plants and cannabis processing products,which can provide technical support for the detection of industrial cannabis plants and cannabis processing products in the laboratory.