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UPLC-MS/MS法测定红景天提取物中6种活性成分的含量 被引量:6

Quantification of six active ingredients in Rhodiola extract by UPLC-MS/MS
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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.
出处 《国际药学研究杂志》 CAS CSCD 北大核心 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)
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 UPLC-MS/MS Rhodiola extract salidroside rhodiosin rhodionin herbacetin kaempferol quercetin
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