DART-MS法快速检测姜黄属中药中姜黄素类化合物的适用性研究  

Rapid detection of applicability of curcuminoids in Curcuma using DART-MS

作　　者：罗霄 肖思远 张良 俞佳 梁恒兴 李及 代琪 李锐[2,4] 肖洪涛 LUO Xiao;XIAO Siyuan;ZHANG Liang;YU Jia;LIANG Hengxing;LI Ji;DAI Qi;LI Rui;XIAOHongtao(Key Laboratory of Quality Monitoring and Evaluation of Traditional Chinese Medicinal Materials,National Medical Products Administration,Chengdu Institute for Drug Control,Chengdu 610045,China;State Key Laboratory of Southwestern Chinese Medicine Resources,Chengdu University of Traditional Chinese Medicine,Chengdu 611137,China;Pharmacy Department of Sichuan Cancer Hospital,Chengdu 610072,China;Sichuan Jinhong Keyou Biotechnology Co.,Ltd.,Chengdu 611137,China;Luzhou Laojiao Group Co.,Ltd.,Luzhou 646000,China)

机构地区：[1]成都市药品检验研究院国家药品监督管理局中药材质量监测评价重点实验室,四川成都610045 [2]成都中医药大学西南特色中药资源国家重点实验室,药学院,四川成都611137 [3]四川省肿瘤医院药学部,四川成都610072 [4]四川锦弘科优生物科技有限责任公司,四川成都611137 [5]泸州老窖股份有限公司,四川泸州646000

出　　处：《中草药》2024年第15期5256-5263,共8页Chinese Traditional and Herbal Drugs

基　　金：国家重点研发计划-中医药现代化专项(2023YFC3504101);国家自然科学基金面上项目(82073994);成都中医药大学杏林学者学科人才科研提升计划(QJJJ2021002)。

摘　　要：目的建立实时直接分析质谱(direct analysis in real-time-mass spectrometer,DART-MS)法检测姜黄属中药中姜黄素类化合物的分析方法,并探究该方法在中药领域应用的可行性。方法利用DART-MS技术,通过单因素实验,优化进样速度、格栅电压、提取溶剂等实验参数条件,获得最佳检测限。与采用超高效液相色谱-电喷雾串联质谱(ultra performance liquid chromatography-electric spray ion source-mass spectrometer,UPLC-ESI-MS)技术检测的结果作比较,并进行方法学验证,以此评价采用DART-MS技术进行快速检测姜黄素类化合物的可行性。结果优化后的DART检测条件:电离源气体温度300℃,格栅电压(grid voltage,GV)100 V,进样速度0.2 mm/s,并以60%丙酮水溶液作为提取剂,以获得最佳信号强度。结果表明,在负离子模式下,姜黄素(curcumin,CUR)、去甲氧基姜黄素(demethoxycurcumin,DMC)、双去甲氧基姜黄素(bisdemethoxycurcumin,BDMC)的标准曲线呈现良好线性关系,检测限分别为0.08、0.10、0.07 ng/mL,定量限分别为0.22、0.34、0.19 ng/mL,3种化合物的平均回收率处于98.75%~100.61%,相对标准偏差(relative standard deviation,RSD)均小于5%。采用DART-MS和UPLC-ESI-MS对3种姜黄素检测的结果一致。结论该方法精确度高、准确度高、重复性好,能快速、准确、有效地检测姜黄属中药中姜黄素类化合物,在中药等领域具有潜在的应用价值。Objective To establish a method using direct analysis in real-time-mass spectrometer(DART-MS)for detecting curcuminoids in Curcuma,and explore the feasibility of the method in the field of traditional Chinese medicine.Methods By using DART-MS technology and conducting single-factor experiments,the experimental parameters such as injection speed,grid voltage(GV),and extraction solvent were optimized to obtain the optimal limit of detection.Comparing the results detected by ultra performance liquid chromatography-electric spray ion source-mass spectrometer(UPLC-ESI-MS)technology and conducting methodological validation to evaluate the feasibility of using DART-MS technology for rapid detection of curcuminoids.Results To obtain the optimal signal intensity,the optimized DART detection conditions are as follows:the ion source gas temperature is 300℃,the GV is 100 V,the sample injection speed is 0.2 mm/s,and a 60%acetone aqueous solution is used as the extraction solvent.The results showed that in negative ion mode,the standard curves of curcumin(CUR),demethoxycurcumin(DMC),and bisdemethoxycurcumin(BDMC)showed a good linear relationship,with detection limits of 0.08,0.10,and 0.07 ng/mL,and quantification limits of 0.22,0.34,and 0.19 ng/mL,respectively.The average recovery rates of the three compounds were between 98.75%and 100.61%,and the relative standard deviation(RSD)was less than 5%.The results of detecting three curcuminoids using DART-MS and UPLC-ESI-MS are almost consistent.Conclusion The method has high precision,high accuracy and good repeatability,and can quickly,accurately and effectively detect curcuminoids in Curcuma,which has potential application value in traditional Chinese medicine and other fields.

关 键 词：姜黄素类化合物 姜黄素 去甲氧基姜黄素 双去甲氧基姜黄素 实时直接分析质谱 超高效液相色谱-电喷雾串联质谱 快速检测 

分 类 号：R284.1[医药卫生—中药学]