摘要
建立了薄层色谱-高效液相色谱-四极杆飞行时间质谱法联用技术(TLC-HPLC-QTOF-M S)快速鉴定柑橘提取物消毒液中桔皮素、蜜橘黄素、新橙皮苷和柚皮苷4种活性物质并测定其含量的方法。样品经氯仿-丙酮洗脱剂梯度洗脱,TLC检识,半制备HPLC纯化,HPLCM S/M S鉴定及HPLC含量测定。结果表明,以氯仿-丙酮(3:1,V/V)作为展开剂分离效果最好。以甲醇-水(7:3,V/V)作为流动相测定桔皮素和蜜橘黄素的含量,以甲醇-0.2%乙酸(13:7,V/V)作为流动相对柚皮苷和新橙皮苷进行定性和定量分析,分离度及峰形最佳。方法测定桔皮素、蜜橘黄素、新橙皮苷和柚皮苷含量的相关系数均大于0.999,检测限分别为:0.3,0.1,0.4,1.2μg/m L,相对标准偏差分别为1.9%,1.9%,2.2%,1.5%,平均回收率分别为97.0%,103.5%,97.8%,100.1%。方法可用于柑橘提取物消毒液质量控制。
A new method based on TLC-HPLC-Q-TOF-MS was established to rapidly identify hesperetin, nobiletin, neohesperidin and naringin in disinfectant containing extracts of citrusand determinate their contents. The samples were gradiently eluted with chloroform-acetone, then identified by TLC, purified by semi-preparative HPLC, identified by HPLC-MS/MS and determined by HPLC. The results showed that the best conditions were as follows： unfolding agents （chloroform： acetone = 3： 1, V/V）, mobile phase of determinating the contents of hesperetin and nobiletin （ Methanol ： water = 70： 30, V/V）, mobile phase of qualitative and quantitative analysis of naringin and neohesperidin： （ methanol ： 0. 2% acetic acid = 65：35, V/V）. The correlation coefficients of the method for determination of hesperetin, nobiletin, naringin and neohesperidinwere higher than 0.999, the detection limits were 0. 3, 0. 1,0. 4, 1.2 g/mL, the relative standard deviations were 1.9%, 1.9%, 2. 2% and 1.5%, and the average recoveres were 97.0%, 103. 5%, 97. 8%, 100. 1%, respectively. This method can be used for the quality control of disinfectant containing extracts of citrus.
作者
袁志鹰
周晓倩
张梦通
周小江
曾光
黄惠勇
朱建平
邓文祥
YUAN Zhi-ying;ZHOU Xiao-qian;ZHANG Meng-tong;ZHOU Xiao-jiang;ZENG Guang;HUANG Hui-yong;ZHU Jian-ping;Jlan-ping;DENG Wen-xiang(Hunan University of Chinese Medicine,Changsha 410208;Hunan Engineering Technology Center of Standardization and Function of Technology Center Chinese Herbal Decoction Pieces,Changsha 410208;Hunan Engineering of Edible Homologous Functional Food,Changsha 410208)
出处
《分析试验室》
CAS
CSCD
北大核心
2018年第9期993-997,共5页
Chinese Journal of Analysis Laboratory
基金
国家自然科学基金青年项目(81403206)
湖南省科技厅社会发展项目(2014SK3042)
湖南省教育厅优秀青年项目(2014B131)
长沙市科技局重点项目(K1406032-11)
中医药防治重症肝炎临床防治中心开放基金项目(ZZGY17)
中医药防治重症肝炎临床防治中心开放基金项目(ZZGY16)资助
