热淋清颗粒中5个成分的UPLC-MS/MS法测定

Determination of Five Components in Relinqing Granules by UPLC-MS/MS

建立了超高效液相色谱串联质谱法同时测定热淋清颗粒中的没食子酸、原儿茶酸、槲皮苷、杨梅苷和陆地棉苷。采用WatersBEHC18色谱柱，以0．1％甲酸乙腈溶液．0．1％甲酸水溶液为流动相，梯度洗脱。采用电喷雾离子源进行正负离子模式同步检测，多反应监测模式（MRM）用于定量测定。没食子酸、原儿茶酸、槲皮苷、杨梅苷和陆地棉苷分别在2．708～219．355、0．116～9．426、0．081～6．581、0．047～3．819和0．055～4．452μg／ml浓度范围内线性关系良好，平均回收率为98．94％～102．16％，RSD〈3％。热淋清颗粒中上述5个成分的总量为30．85～40．71mg／包。

An UPLC-MS/MS method was established for the determination of gallic acid, protocatechuic acid, quercitrin, myricitrin and hirsutrin in Relinqing granules. A Waters BEH C18 column was used with the mobile phase of 0.1% formic acid acetonitrile solution-0.1% formic acid aqueous solution by gradient elution. Multiple-reaction monitoring （MRM） scanning mode was employed for quantification with switching electrospray ion source polarity in positive/negative mode. The calibration curves for gallic acid, protocatechuic acid, quercitrin, myricitrin and hirsutrin were linear in the concentration ranges of 2.708 - 219.355, 0.116 - 9.426, 0.081 - 6.581, 0.047 - 3.819 and 0.055 - 4.452 μg/ml. Their average recoveries were 98.94 % - 102.16 %, with RSDs less than 3 %. The total content of the five components in Relinqing granules was 30.85 - 40.71 mg per package.