UPLC-MS/MS法测定红景天提取物中6种活性成分的含量  

Quantification of six active ingredients in Rhodiola extract by UPLC-MS/MS

作　　者：赵亮[1] 齐特[1] 葛贝康[1] 徐平湘[1,2] 薛明[1,2] 

机构地区：[1]首都医科大学基础医学院药理学系,北京100069 [2]首都医科大学生物医学检测技术与仪器北京实验室,北京100069

出　　处：《国际药学研究杂志》2016年第5期975-979,共5页Journal of International Pharmaceutical Research

基　　金：国家自然科学基金资助项目(81573683)

摘　　要：目的：建立并验证同时测定红景天（Rhodiola）提取物中红景天苷、红景天素、草质素苷、草质素、山柰酚和槲皮素6种活性成分含量的UPLC-MS/MS方法。方法色谱条件：采用Zorbax Eclipse plus C18色谱柱（100 mm×2.1 mm，3.5μm）；0.2%甲酸水-乙腈为流动相，洗脱方式为梯度洗脱；流速为0.4 ml/min；柱温为25℃。质谱条件：采用电喷雾离子源（ESI），负离子检测，扫描方式为多反应监测模式（MRM）。结果6种活性成分分别在10～20000，10～4000、10～4000、5～2000、10～2000和5～2000 ng/ml之间线性关系良好。仪器精密度RSD＜3.31%，6种活性成分的稳定性RSD＜5.07%，重复性RSD＜4.05%，平均回收率在99.27%～108.91%，RSD均＜4.92%。结论本法可同时测定红景天提取物中6种活性成分含量，具有快速、灵敏度高、专属性好，重复性好的特点。Objective To develop and fully validate an UPLC-MS/MS method for simultaneous quantification of six active in-gredients in Rhodiola extract including salidroside,rhodiosin,rhodionin,herbacetin,kaempferol and quercetin. Methods The chro-matographic separation of the analytes was achieved by using Zorbax Eclipse plus C18 column（2.1 mm×100 mm,3.5μm）. The mobile phase consisted of 0.2%aqueous formic acid and acetonitrile. Analytes were separated using a linear gradient with a flow rate of 0.4 ml/min. The column temperature was set at 25℃. The mass spectrometric conditions were electrospray negative ionization（ESI）and the scan-ning mode was multi reaction monitoring（MRM）. Results The calibration curves of the six active ingredients were linear over 10-20000,10-4000,10-4000,5-2000,10-2000,and 5-2000 ng/ml concentration ranges,respectively. The RSD of the instrument precision was within 3.31%. The current assay was stable and reproducible in quantification of all analytes with RSD within 5.07%and 4.05%,respectively. The average recovery of all analytes was in a range from 99.27%to 108.91%,with an acceptable RSD of no more than 4.92%. Conclusion The UPLC-MS/MS method could be successfully applied to simultaneously quantifying six major active in-gredients in Rhodiola extract with the acceptable specificity,sensitivity and reproducibility.

关 键 词：UPLC-MS/MS 红景天提取物 红景天苷 红景天素 草质素苷 草质素 山柰酚 槲皮素 

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