基于超高效液相色谱-三重四极杆串联质谱法测定9种食品基质中3种大麻素

Determination of Three Cannabinoids in Nine Food Matrices by Ultra-high Performance Liquid ChromatographyTriple Quadrupole Tandem Mass Spectrometry

在优化前处理条件和色谱分离的基础上,建立同时测定橄榄油、牛肉、面包等9种食品中大麻酚、大麻二酚和Δ9-四氢大麻酚的超高效液相色谱-三重四极杆串联质谱测定方法。最终选择用乙腈或甲醇提取,EMR或二乙烯苯-N-乙烯基吡咯烷酮(HLB)固相萃取小柱净化,以甲醇和10 mmol/L乙酸铵溶液为流动相,在BEH C18色谱柱(2.1 mm×50 mm,1.7μm)上分离,用电喷雾电离源(正离子模式),多反应监测模式测定,同位素内标定量。结果表明,该方法在0~200μg/L质量浓度范围内具有良好的线性关系,相关系数均大于0.998。方法的检出限(信噪比3)和定量限(信噪比10)分别为3μg/kg和10μg/kg。在空白样品中进行3个水平(1、2、10倍定量限)的加标回收实验(n=6),3种大麻素化合物的回收率为71.7%~108.5%,相对标准偏差为4.6%~12.4%。本实验建立的方法稳定性好,灵敏度高,能够满足常见食品基质中大麻素的检测要求。

In this study,a method based on ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry(UPLC-MS-MS)was developed for the simultaneous determination of cannabinol,cannabidiol andΔ9-tetrahydrocannabinol in nine food matrices such as olive oil,beef and bread.The samples were extracted with acetonitrile or methanol and purified using an EMR or HLB solid-phase extraction(SPE)cartridge.The analytes were separated on a BEH C18 column(2.1 mm×50 mm,1.7μm)using methanol and 10 mmol/L ammonium acetate in water as the mobile phase,ionized using an electrospray ionization(ESI)source in the positive ion mode,detected in the multiple reaction monitoring(MRM)mode,and quantified by the internal standard method.The calibration curves for all analytes showed good linearity in the concentration range of 0–200μg/L,with correlation coefficients greater than 0.998.The limits of detection(at a signal to noise ratio of 3)and quantitation(at a signal to noise ratio of 10)were 3 and 10μg/kg,respectively.The average recoveries for negative samples spiked at three concentration levels(1,2,10 times of the limit of quantitation)were 71.7%–108.5%,with relative standard deviations(RSDs)of 4.6%–12.4%(n=6).In summary,this method has good stability and high sensitivity,and is suitable for simultaneous determination of the three cannabinoids in common food matrices.