响应面优化分散固相萃取-超高效液相色谱-串联质谱法测定膨化食品中3种大麻酚类化合物的含量  

Determination of 3 Cannabinols in Puffed Foods by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry with Dispersive Solid Phase Extraction Optimized by Response Surface Methodology

作　　者：郝志明 冯奎 肖艳萍[1] 李冬梅[1] 李宝玉[1] 姚小华 赵培静 吴燕燕[4] HAO Zhiming;FENG Kui;XIAO Yanping;LI Dongmei;LI Baoyu;YAO Xiaohua;ZHAO Peijing;WU Yanyan(Guangdong Agriculture Industry Business Polytechnic,Guangzhou 524088,China;Foshan Xiangshang Food Technology Co.,Ltd.,Foshan 528139,China;Guangdong Huawei Testing Co.,Ltd.,Guangzhou 510700,China;Key Laboratory of Aquatic Product Processing,Ministry of Agriculture and Rural Affairs of the People's Republic of China,South China Sea Fisheries Research Institute,Chinese Academy of Fishery Sciences,Guangzhou 510300,China)

机构地区：[1]广东农工商职业技术学院,广州524088 [2]佛山象尚食品科技有限公司,佛山528139 [3]广东省华微检测股份有限公司,广州510700 [4]中国水产科学研究院南海水产研究所农业农村部水产品加工重点实验室,广州510300

出　　处：《理化检验（化学分册）》2024年第10期993-999,共7页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家海水鱼产业技术体系(CARS-47);广东农工商职业技术学院/佛山象尚食品科技有限公司产学研项目(02.0570)。

摘　　要：采用单因素和响应面法优化净化剂和提取溶剂用量,提出了题示方法。取2 g粉碎后的膨化食品样品,依次加入10 mL水、10 mL乙腈、4 g无水硫酸镁和1 g氯化钠,涡旋振荡15 min,离心5 min。取2 mL上清液置于含有200 mg十八烷基硅烷键合硅胶(C_(18))和30 mg N-丙基乙二胺(PSA)的离心管中,涡旋2 min,离心5 min,上清液过0.22μm滤膜,滤液采用超高效液相色谱-四极杆/飞行时间质谱法(UHPLC-Q-TOF/MS)测定。滤液中的大麻二酚、大麻酚、四氢大麻酚在Agilent Extend C_(18)色谱柱上用不同体积比的0.1%(体积分数)氨水溶液和乙腈的混合溶液梯度洗脱分离,电喷雾离子源负离子模式电离,基质匹配法定量。结果显示:建立的三因素三水平响应面模型为二次回归方程,相关系数为0.9949,最优条件(C_(18)、PSA和乙腈用量分别为200 mg、30 mg和10 mL)下考察指标四氢大麻酚的回收率试验值(94.1%)和预测值(93.6%)吻合;3种目标物的质量浓度在5.0~200μg·L^(-1)内和对应的母离子峰面积呈线性关系,检出限(3S/N)均为10.0μg·kg^(-1);对阴性米饼进行3个浓度水平的加标回收试验,回收率为81.9%~94.1%,测定值的相对标准偏差(n=6)为3.9%~7.3%。方法用于米饼、饼干、薯片样品的分析,在1个进口饼干样品中检出了大麻酚(27.8μg·kg^(-1))、大麻二酚(113μg·kg^(-1))和四氢大麻酚(30.6μg·kg^(-1)),其他样品均未检出这3种目标物。The method mentioned by the title was proposed after optimizing amounts of purification agent and extraction solvent by single factor and response surface methodology.The 2 g of crushed puffed food sample was taken,and 10 mL of water,10 mL of acetonitrile,4 g of anhydrous magnesium sulfate and 1 g of sodium chloride were added in sequence.The mixture was vortexed for 15 min and centrifuged for 5 min,and 2 mL of supernatant was taken and placed into a centrifuge tube containing 200 mg of octadecylsilane bonded silica gel(C_(18))and 30 mg of N-propylethylenediamine(PSA).After vortexing for 2 min,and centrifuging for 5 min,the supernatant was passed through a 0.22μm filter membrane,and the filtrate was determined by ultrahigh performance liquid chromatography-quadrupole/time-of-flight mass spectrometry(UHPLC-Q-TOF/MS).Cannabidiol,cannabinol and tetrahydrocannabinol in the filtrate were separated by gradient elution with mixed solutions of 0.1%(volume fraction)aqueous ammonia solution and acetonitrile at different volume ratios on the Agilent Extend C_(18) chromatographic column,ionized by negative ion mode of electrospray ion source,and quantified by matrix matching method.It was shown that the established three-factor three-level response surface model was a quadratic regression equation with correlation coefficient of 0.9949.Under the optimal conditions(C_(18),PSA,and acetonitrile amounts of 200 mg,30 mg,and 10 mL,respectively),the experimental value(94.1%)and predicted value(93.6%)of the tetrahydrocannabinol recovery were consistent.Linear relationships between values of the mass concentrations of the 3 targets and peak areas of the corresponding parent ions were kept in the range of 5.0-200μg·L^(−1),with the same detection limit(3S/N)of 10.0μg·kg^(−1).Test for the spiked recovery at the 3 concentration levels was conducted on negative rice cakes,giving recoveries in the range of 81.9%-94.1%,and RSDs(n=6)of the determined values ranged from 3.9%to 7.3%.The proposed method was used for the analysis of sam

关 键 词：分散固相萃取 超高效液相色谱-四极杆/飞行时间质谱法 膨化食品 大麻酚类化合物 响应面 

分 类 号：O657.63[理学—分析化学]