超高效液相色谱质谱法测定饼干中3种大麻酚  

Determination of Three Cannabinoids in Biscuits by Ultra⁃high Performance Liquid Chromatography⁃Mass Spectrometry

作　　者：张闯 赵孔祥 张敏 王利强 ZHANG Chuang;ZHAO Kongxiang;ZHANG Min;WANG Liqiang(Tianjin Customs Industrial Product Safety Technology Center,Tianjin 300457,China;Tianjin Customs Animal and Plant Food Testing Center,Tianjin 300457,China)

机构地区：[1]天津海关工业产品安全技术中心,天津300457 [2]天津海关动植物食品检测中心,天津300457

出　　处：《食品研究与开发》2024年第9期159-165,共7页Food Research and Development

基　　金：国家重点研发计划项目(2022YFF1100804)。

摘　　要：使用超高效液相色谱-串联质谱法,建立饼干中大麻酚、大麻二酚和四氢大麻酚的测定方法。样品经乙腈醋酸(99+1)提取,加入醋酸体系盐包超声离心后,再加入吸附剂离心。采用0.1%甲酸水溶液和甲醇为流动相,梯度洗脱,通过C18色谱柱分离,大气压化学电子源(atmospheric pressure chemical ionization,APCI)正离子多反应模式监测。通过考察不同种类提取溶剂、超声时间、萃取盐包组成、吸附剂组成的目标化合物回收率,确定最优前处理方式。结果表明:大麻酚、大麻二酚、四氢大麻酚在2~100 ng/mL时呈现良好线性关系,相关系数(R2)均大于0.999,方法检出限0.01 mg/kg,定量限0.02 mg/kg。低、中、高3个浓度加标回收试验,大麻酚回收率为80.3%~91.1%,相对标准偏差(relative standard deviation,RSD)为2.4%~6.5%,大麻二酚回收率为78.4%~88.5%,RSD为2.9%~7.5%,四氢大麻酚回收率为81.5%~91.3%,RSD为2.6%~6.8%。该方法适用于饼干中大麻酚、大麻二酚和四氢大麻酚的检测。A method for the determination of cannabinol,cannabidiol,and tetrahydrocannabinol in biscuits using ultra⁃high performance liquid chromatography tandem mass spectrometry technology was established.The sample was extracted with acetonitrile⁃acetic acid(99+1),added to the acetic acid system for salt pack⁃age ultrasonic centrifugation,and then added to the adsorbent for centrifugation.Using a 0.1%formic acid aqueous solution and methanol as the mobile phase,gradient elution was performed,separated by C18 chro⁃matographic column,and monitored by atmospheric pressure chemical ionization(APCI)positive ion multiple reaction mode.By examining different types of extraction solvents,ultrasonic time,salt package system selec⁃tion,and target compound recovery rate of adsorbent composition,the optimal pre⁃treatment method was deter⁃mined.The results showed that cannabinol,cannabidiol,and tetrahydrocannabinol exhibited a good linear re⁃lationship in the range of 2-100 ng/mL,with correlation coefficients(R2)all greater than 0.999.The limit of detection of the method was 0.01 mg/kg,and the limit of quantitation was 0.02 mg/kg.In the low,medium,and high concentration spiked recovery experiment,the recovery rate of cannabinol ranged from 80.3%to 91.1%,with a relative standard deviation(RSD)of 2.4%-6.5%.The recovery rate of cannabidiol ranged from 78.4%to 88.5%,with an RSD of 2.9%-7.5%.The recovery rate of tetrahydrocannabinol ranged from 81.5%to 91.3%,with an RSD of 2.6%-6.8%.This method is fast,simple,highly accurate,has good reproducibility,and is suitable for the detection of cannabidiol,cannabidiol,and tetrahydrocannabidiol in biscuits.

关 键 词：大麻酚类物质 QUECHERS 饼干 液相色谱质谱 大气压化学电子源 

分 类 号：O657.63[理学—分析化学] TS213.22[理学—化学]