超高效液相色谱-高分辨质谱法分析不同食品基质中多种新型合成大麻素  

Determination of several novel synthetic cannabinoids in different food matrices by ultra-high performance liquid chromatography-high resolution mass spectrometry

作　　者：郭思言 蔡翔宇 郑文 景渝 何梦婷 程妮郦 李晓华 郗存显 李光满 刘高峰 廖海霞 GUO Siyan;CAI Xiangyu;ZHENG Wen;JING Yu;HE Mengting;CHENG Nili;LI Xiaohua;XI Cunxian;LI Guangman;LIU Gaofeng;LIAO Haixia(Technical Center of Chongqing Customs,Chongqing,400020,China;Technical Center of Nanning Customs;Chongqing Customs;The Experimental High School Attached to UESTC)

机构地区：[1]重庆海关技术中心,重庆400020 [2]南宁海关技术中心 [3]重庆海关 [4]电子科技大学实验中学

出　　处：《质量安全与检验检测》2024年第1期8-15,共8页QUALITY SAFETY INSPECTION AND TESTING

基　　金：海关总署科研项目(2021HK206)。

摘　　要：建立了一种超高效液相色谱-高分辨质谱法分析不同食品中新型合成大麻素的检测方法,利用高分辨质谱对合成大麻素类化合物特征碎片分析,建立二级谱图库。样品经甲醇提取,沉淀蛋白后,提取液过HLB固相萃取柱净化,C18色谱柱分离,以甲醇-含0.1%甲酸的2 mmol/L乙酸铵溶液为流动相梯度洗脱,电喷雾正离子模式扫描,全扫描-自动触发二级扫描模式监测,用基质配标法消除基质效应,外标法定量。该方法在1~500μg/L浓度范围内线性相关系数(R^(2))均>0.999。饼干和蛋糕中大麻素类化合物的检测限(LOD)为3μg/kg,定量限(LOQ)为10μg/kg,饮料中大麻素类化合物的LOD为0.6μg/kg,LOQ为2μg/kg。大麻素类化合物在3种不同食品基质中进行3水平的加标回收,平均加标回收率为75.1%~106.7%。相对标准偏差(RSD)为2.5%~10.3%(n=6)。结果表明,该方法精密度好、灵敏度高,回收率好,可以满足常见食品基质中新型合成大麻素类物质的同时测定,利用二级碎片谱图库可实现对合成大麻素类物质的有效鉴定。A ultra-high performance liquid chromatography-high resolution mass spectrometry method was developed to simultaneously determine the levels of natural cannabinoids and synthetic cannabinoid compounds in various food samples.Additionally,a high-resolution mass spectrometry was utilized for the analysis of characteristic fragment ions of cannabinoid compounds,leading to the establishment of a secondary spectral library.The samples were extracted with methyl alcohol,purified using HLB solid-phase extraction column,separated by C18 chromatographic column,and eluted with a gradient of methanol and 2 mmol ammonium acetate solution containing 0.1%formic acid.The analysis was performed by external standard method using electrospray ionization in positive ion mode,employing multiple reaction monitoring mode for detection,and matrix matching was employed to eliminate matrix effects.The developed method exhibited excellent linearity with correlation coefficients(R^(2))greater than 0.999 across the concentration range of 1-500μg/L.The limit of detection(LOD)for cannabinoid compounds in biscuits and cakes was determined to be 3μg/kg,with a limit of quantification(LOQ)of 10μg/kg.In beverages,the LOD for cannabinoid compounds was found to be 0.6μg/kg,with a LOQ of 2μg/kg.The three-level spiked recovery of cannabinoid compounds in three different food matrices,namely biscuits,cakes,and beverages,yielded average recovery rates ranging from 75.1%to 106.7%.The relative standard deviation(RSD)ranged from 2.5%to 10.3%(n=6),indicating excellent precision and sensitivity of the method.These results demonstrate that the method is capable of simultaneous determination of cannabinoid compounds in commonly encountered food matrices,and the utilization of the secondary spectral library enables effective identification of these compounds.

关 键 词：新型合成大麻素 超高效液相色谱 高分辨质谱 食品 

分 类 号：O657.63[理学—分析化学]