解吸附电晕束电离质谱法快速测定黄精中的薯蓣皂苷元  

Rapid Determination of Diosgenin in Polygonati rhizoma by Desorption Corona Beam Ionization Mass Spectrometry

作　　者：陈诗丽 闵可 杨蓉[1] 罗玮[1] 谢小玉 陈波[1] 马铭[1] CHEN Shi-li;MIN Ke;YANG Rong;LUO Wei;XIE Xiao-yu;CHEN Bo;MA Ming(Key Laboratory of Phytochemical R&D of Hunan Province,Key Laboratory of Chemical Biology&Traditional Chinese Medicine Research Ministry of Education of China,Hunan Normal University,Changsha 410081,China)

机构地区：[1]湖南师范大学化学生物学及中药分析教育部重点实验室,植化单体开发与利用湖南省重点实验室,中国长沙410081

出　　处：《湖南师范大学自然科学学报》2022年第5期136-143,共8页Journal of Natural Science of Hunan Normal University

基　　金：国家自然科学基金项目(21775041,21775040)。

摘　　要：应用解吸附电晕束质谱法(DCBI-MS)快速定性定量分析传统中药黄精中的薯蓣皂苷元,通过质谱碎片离子探究薯蓣皂苷元的裂解规律。采用DCBI-MS技术在选择离子监测(SIM)正离子模式下工作,氦气流量、放电电压和解吸附温度分别设置为1.0 L·min^(-1),1.8 kV和320℃。样品上样体积为20μL。以甲睾酮作为内标,薯蓣皂苷元在0.5~10.0 mg·L^(-1)具有良好的线性相关性,相关系数R 2为0.9993。检测的精密度为15%,检出限(LOD)和定量限(LOQ)分别为0.1和0.4 mg·L^(-1)。加标回收率范围为90.0%~106.8%。采用DCBI-MS法和传统高效液相色谱(HPLC)法对8批次黄精中的薯蓣皂苷元含量进行测定,两种方法得到的测定结果无显著性差异。本研究建立的黄精中薯蓣皂苷元的DCBI-MS检测方法拥有无需色谱分离过程、试剂消耗少、简单快速的优点,可作为黄精中薯蓣皂苷元快速定性定量分析的新策略。Desorption corona beam ionization mass spectrometry(DCBI-MS)has been developed for a rapid qualitative and quantitative analysis of diosgenin in traditional Chinese medicine,Polygonati rhizoma.The MS fragmentation mechanism of diosgenin has been explored by fragmentary ions.DCBI-MS experiments were performed in the positive ion mode of selective ion monitoring(SIM)with the helium flow rate,high voltage discharge and desorption temperature set at 1.0 L·min^(-1),1.8 kV and 320℃,respectively.The sample injection volume was 20μL.With methyltestosterone as the internal standard,a good linear regression equation was obtained in the concentration range of from 0.5 to 10.0 mg·L^(-1) for diosgenin,and the correlation coefficient R^( 2) was 0.9993.The relative standard deviation(RSD)was 15%,and the limits of detection(LOD)and quantification(LOQ)of diosgenin were 0.1 and 0.4 mg·L^(-1),respectively.The spiked recovery range was from 90.0%to 106.8%.For comparison,the DCBI-MS method and traditional HPLC method were used to determine the contents of diosgenin in 8 batches of Polygonati rhizoma,and the results showed no significant difference.In this study,the established DCBI-MS method for the analysis of diosgenin in Polygonati rhizoma has advantages of no chromatographic separation process,less reagent consumption,simplicity and rapidity,which is a new strategy for the rapid qualitative and quantitative analysis of diosgenin in Polygonati rhizoma.

关 键 词：解吸附电晕束电离质谱法 黄精 薯蓣皂苷元 高通量分析 

分 类 号：R284.1[医药卫生—中药学] O657.63[医药卫生—中医学]