协日嘎-4味散成分组成分析及6种成分含量测定  

Analysis of component composition and content determination of six constituents for Xeriga-4 Powder

作　　者：李君 王跃武[1,2] 张谦 翠平[3] 叶日贵 吉日木巴图[3] LI Jun;WANG Yue-wu;ZHANG Qian;CUI Ping;YE Ri-gui;Ji-ri-mu-ba-tu(College of Pharmacy,Inner Mongolia Medical University,Hohhot 010110,China;Engineering Research Center for New Pharmaceutical Screening,Inner Mongolia Medical University,Hohhot 010110,China;Innovation Center for Ethnic Medicines,Inner Mongolia Medical University,Hohhot 010110,China)

机构地区：[1]内蒙古医科大学药学院,内蒙古呼和浩特010110 [2]内蒙古医科大学新药筛选工程研究中心,内蒙古呼和浩特010110 [3]内蒙古医科大学民族医药创新中心,内蒙古呼和浩特010110

出　　处：《中成药》2024年第1期14-22,共9页Chinese Traditional Patent Medicine

基　　金：内蒙古自治区自然科学基金资助项目(2022LHQN08001);内蒙古自治区卫生健康委医疗卫生科技计划项目(202201186);内蒙古自治区高等学校科学研究项目(NJZY22655);内蒙古医科大学“致远”人才项目(ZY0301015);内蒙古医科大学面上项目(YKD2022MS038)。

摘　　要：目的分析协日嘎-4味散成分组成,并测定黄柏碱、绿原酸、栀子苷、小檗碱、芦丁、姜黄素的含量。方法高效液相色谱-四级杆/静电场轨道阱高分辨质谱(HPLC-Q-Exactive-MS)定性分析采用Agilent ZORBAX SB-Aq色谱柱(4.6 mm×150 mm,5μm);流动相甲醇-0.1%甲酸,梯度洗脱;体积流量0.35 mL/min;柱温35℃;电喷雾离子源;正负离子扫描。高效液相色谱串联三重四级杆质谱(HPLC-MS/MS)定量分析采用Shim-pack GIST-HP C_(18)色谱柱(2.1 mm×100 mm,3μm);流动相甲醇-0.1%甲酸;体积流量0.25 mL/min;柱温35℃;电喷雾离子源;正负离子扫描;多反应监测模式。结果共鉴定出65种成分,包括19种生物碱、13种有机酸、13种黄酮、7种姜黄素、6种环烯醚萜、4种脂肪酸、2种醛、1种氨基酸。6种成分在各自范围线性关系良好(r≥0.9991),平均加样回收率96.44%~102.37%,RSD 2.05%~3.74%。结论本研究可为协日嘎-4味散的质量控制提供参考。AIM To analyze the component composition of Xeriga-4 Powder,and to determine the contents of phellodendrine,chlorogenic acid,gardenoside,berberine,rutin and curcumin.METHODS The high performance liquid chromatography-Q-exactive orbitrap mass spectrometry(HPLC-Q-Exactive-MS)qualitative analysis was performed on a 35℃thermostatic Agilent ZORBAX SB-Aq column(4.6 mm×150 mm,5μm),with the mobile phase comprising of methanol-0.1%formic acid flowing at 0.35 mL/min in a gradient elution manner,and electron spray ionization source was adopted in positive and negative ion scanning.High performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS)quantitative analysis was performed on a 35℃thermostatic Shim-pack GIST-HP C_(18) column(2.1 mm×100 mm,3μm),with the mobile phase comprising of methanol-0.1%formic acid flowing at 0.25 mL/min in a gradient elution manner,and electron spray ionization source was adopted in positive and negative ion scanning with multiple reaction monitoring mode.RESULTS Total 65 constituents were identified,containing 19 alkaloids,13 organic acids,13 flavonoids,7 curcumins,6 iridoids,4 fatty acids,2 aldehydes,and 1 amino acid.Six constituents showed good linear relationships within their own ranges(r≥0.9991),whose average recoveries were 96.44%-102.37%with the RSDs of 2.05%-3.74%.CONCLUSION This study can provide a reference for the quality control for Xieriga-4 Powder.

关 键 词：协日嘎-4味散 成分组成 化学成分 含量测定 高效液相色谱-四级杆/静电场轨道阱高分辨质谱(HPLC-Q-Exactive-MS) 高效液相色谱串联三重四级杆质谱(HPLC-MS/MS) 

分 类 号：R284[医药卫生—中药学]