LC-MS-MS测定配伍黄柏对知母中4种有效成分含量的影响  

Effects of Phellodendri Cortex on Contents of Four Ingredients from Anemarrhenae Rhizoma Determined by LC-MS-MS

作　　者：邱昆成 孙振刚[1] 何倩梅[1] 李丹[1] 刘奕明[1] 林爱华[1] 

机构地区：[1]广州中医药大学附属广东省中医院,广州510120

出　　处：《中国实验方剂学杂志》2016年第14期84-88,共5页Chinese Journal of Experimental Traditional Medical Formulae

基　　金：广东省科技计划项目(2014A020221115);广东省中医院中医药科学技术研究专项(YN2014ZHR206)

摘　　要：目的:建立高效液相色谱串联质谱法(LC-MS-MS)测定知母黄柏药对中芒果苷、新芒果苷、知母皂苷AⅢ和知母皂苷BⅡ的含量,研究不同配伍比例对4种成分含量的影响。方法:采用ZORBAX Eclipse XDB-C_(18)色谱柱(2.1 mm×150 mm,3.5μm),柱温30℃,流动相0.1%甲酸水-乙腈,流速0.25 m L·min^(-1),梯度洗脱;质谱条件为电喷雾(ESI)离子源,负离子多反应离子监测(MRM)用于定量测定。结果:芒果苷、新芒果苷、知母皂苷AⅢ和知母皂苷BⅡ分别在5.05~404,5.3~424,5.05~404,20.8~1 664μg·L^(-1)线性关系良好(r≥0.999);平均回收率分别为100.6%,99.2%,99.1%,98.5%。知母单煎时芒果苷、知母皂苷AⅢ含量最高;新芒果苷在知柏配伍比例1∶1时含量最高;知母皂苷BⅡ的含量各配伍比例没有明显差异。结论:该方法快速、准确,适用于知母黄柏中4种成分的含量测定。知母与黄柏配伍比例不同,芒果苷、新芒果苷、知母皂苷AⅢ的含量不同,配伍黄柏时对知母成分含量有影响。Objective： To establish a liquid chromatography-mass spectrometry-mass spectrometry （LC- MS-MS） method to study the effects of Phellodendri Cortex （CP） on the contents of four ingredients （mangiferin, neomangiferin, timosaponin A Ⅲ and timosaponin B Ⅱ ） from Anemarrhenae Rhizoma （RA）. Method： Chromatographic separation was carried out on ZORBAX Eclipse XDB-C18 column （2. 1 mm × 150 mm, 3.5 μm） , with 0. 1% formic acid-acetonitrile as the mobile phase for gradient elution. The column temperature was 30℃ and the flow rate was 0.25 mL · min-1. The quantification of the analytes was performed by mass spectrometry with electrospray ionization （ESI） under negative ion multiple reaction monitoring （MRM） mode. Result： Mangiferin, neomangiferin, timosaponin A m and timosaponin B Ⅱ had good linear relationship between 5.05-404, 5.3-424, 5.05-404, 20. 8-1 664μg · L-1 respectively （ r ≥ 0. 999）. The average recovery rate was 100.6% , 99.2% , 99. 1% and 98.5% , respectively. The contents of mangiferin and timosaponin A m were highest in group RA-CP （1：0）. Neomangiferin content in group RA-CP （1：1 ） was higher than that in other groups. Timosaponin BⅡ content was similar in each group. Conclusion： The method is rapid, accurate and reliable, and has been successfully used to the quantification of four compounds above mentioned in RA-CP. The contents mangiferin, neomangiferin and timosaponin AⅢ can be affected by the different RA-CP compatibility.

关 键 词：液质联用 芒果苷 新芒果苷 知母皂苷AⅢ 知母皂苷BⅡ 含量测定 

分 类 号：R284.1[医药卫生—中药学]