超高效液相色谱-串联三重四极杆质谱法测定化妆品中3种大麻素

Determination of tetrahydrocannabinol, cannabidiol and cannabinol in cosmetics by ultra performance liquid chromatography-triple quadrupole mass spectrometry

建立了超高效液相色谱-串联三重四极杆质谱法同时测定化妆品中3种特征大麻素的检测方法。样品经乙腈超声提取,采用自制QuEChERS方法净化,然后经过Athena C_(18)-WP色谱柱(2.1 mm×150 mm,3μm)分离,以乙腈-水为流动相,通过优化流动相的洗脱梯度,3种大麻素得到较好的色谱分离。结果表明,大麻酚(Cannabinol,CBN)和大麻二酚(Cannabidiol,CBD)在0.1~10μg/L范围,四氢大麻酚(Tetrahydrocannabinol,THC)在1~100μg/L范围内均呈现较好线性关系,线性相关系数均大于0.999;以3 S/N定为检出限(LOD),10 S/N定为定量限(LOQ),3种大麻素的LOD在0.3~3μg/kg,LOQ在1~10μg/kg;分别在护肤水、乳、霜空白基质中添加大麻素,在1 LOQ、2 LOQ、10 LOQ的加标水平下,采用基质配标法对3种大麻素同时定量分析,3种大麻素的加标回收率为82.3%~108.1%。相对标准偏差(RSD)为1.2%~5.8%(n=6)。该方法稳定性好、灵敏度高,适用于常见化妆品中3种大麻素的定性定量分析。

A method for simultaneous determination of three cannabinoids in cosmetics by ultra performance liquid chromatography-triple quadrupole mass spectrometry was established.The samples were extracted by acetonitrile,purified by QuEChERS method,and then separated by Athena C_(18)-WP column(2.1 mm×150 mm,3μm),using acetonitrile-water as mobile phase.By optimizing the elution gradient of mobile phase,the separation for the three cannabinoids was well achieved.The linear correlation coefficients(r^(2))of cannabinol(CBN)and cannabidiol(CBD)were both greater than 0.999 in the concentration range of 0.1~10μg/L,and the linear correlation coefficient of tetrahydrocannabinol(THC)in the concentration range of 1~100μg/L was greater than 0.999.When 3 S/N was used as the limit of detection(LOD)and 10 S/N was used as the limit of quantification(LOQ),the LOD of the three cannabinoids was 0.3~3μg/kg,and the LOQ was 1~10μg/kg.The matrix matching method was used to quantify the three cannabinoids simultaneously.The recovery rates of the three cannabinoids were 82.3%~108.1%at the standard addition levels of 1 LOQ,2 LOQ and 10 LOQ.The relative standard deviation(RSD)was 1.2%~5.8%(n=6).The results show that the method has good stability and high sensitivity,and is suitable for simultaneous determination of the three cannabinoids in common cosmetics.