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超高效液相色谱-电喷雾串联质谱法同时测定强身片中19种主要活性成分

Simultaneous determination of nineteen major active compounds in Qiangshen tablet by UPLC-ESI-MS/MS.

作者信息

Gao Jinwei, Qiu Ying, Chen Jinmei, Mu Shanxue, Sun Lixin

机构信息

School of Pharmacy, Shenyang Pharmaceutical University, Shenyang, Liaoning, China.

School of Pharmacy, Shenyang Pharmaceutical University, Shenyang, Liaoning, China.

出版信息

J Pharm Biomed Anal. 2016 Sep 5;128:519-527. doi: 10.1016/j.jpba.2016.05.045. Epub 2016 May 26.

Abstract

An ultra high performance liquid chromatography coupled with triple quadrupole mass spectrometry method has been developed to evaluate the quality of a pharmaceutical herbal preparation, Qiangshen tablet, through a simultaneous determination of 19 major active compounds (stachydrine hydrochloride, betaine, gallic acid, sodium danshensu, morroniside, loganin, protocatechuic aldehyde, gardenoside, sweroside, acteoside, paeoniflorin, ginsenoside Re, rosmarinic acid, salvianolic acid B, ginsenoside Rg1, psoralen, isopsoralen, ginsenoside Rb1, paeonol). Chromatographic separation was achieved on an ACQUITY UPLC(®) BEH C18 column (2.1×100mm, 1.7μm) by gradient elution with the mobile phase of 0.1% formic acid aqueous solution (A) and acetonitrile (B). Multiple reaction monitoring (MRM) mode with positive and negative electrospray ionization interface was operated to detect the 19 compounds. All calibration curves showed excellent linear regressions (r>0.999) within the test range. The precision, repeatability and stability of the 19 compounds were below 2.0% in terms of RSD. The recoveries were 97.5-102.2% with RSD of 1.0-1.9% for Qiangshen tablet samples. The method was successfully used for the analysis of samples of Qiangshen tablet. In conclusion, a rapid, sensitive, precise, accurate and reliable UPLC-ESI-MS/MS method has been developed for the simultaneous detection of 19 active compounds with large difference in level of content in the pharmaceutical samples of Qiangshen tablet, which can be applied for the quality control of Qiangshen tablet.

摘要

已开发出一种超高效液相色谱-三重四极杆质谱联用方法,通过同时测定19种主要活性成分(盐酸水苏碱、甜菜碱、没食子酸、丹参素钠、莫诺苷、马钱苷、原儿茶醛、栀子苷、獐牙菜苷、毛蕊花糖苷、芍药苷、人参皂苷Re、迷迭香酸、丹酚酸B、人参皂苷Rg1、补骨脂素、异补骨脂素、人参皂苷Rb1、丹皮酚)来评价一种中药制剂强身片的质量。采用ACQUITY UPLC(®) BEH C18色谱柱(2.1×100mm,1.7μm),以0.1%甲酸水溶液(A)和乙腈(B)为流动相进行梯度洗脱,实现色谱分离。采用正、负离子电喷雾电离接口的多反应监测(MRM)模式检测这19种化合物。所有校准曲线在测试范围内均显示出良好的线性回归(r>0.999)。19种化合物的精密度、重复性和稳定性的相对标准偏差(RSD)均低于2.0%。强身片样品的回收率为97.5 - 102.2%,RSD为1.0 - 1.9%。该方法成功用于强身片样品的分析。总之,已开发出一种快速、灵敏、精确、准确且可靠的UPLC-ESI-MS/MS方法,用于同时检测强身片药物样品中含量差异较大的19种活性成分,可应用于强身片的质量控制。

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