高效液相色谱-质谱联用法同时测定脑心清原料药浸膏及其片剂中的8种有效成分

建立了高效液相色谱-质谱联用（HPLC-MS/MS）同时测定脑心清原料药及其片剂中原儿茶酸、金丝桃苷、山柰酚-3-O-β-D-吡喃葡萄糖苷、山柰酚-3-O-β-D-吡喃半乳糖苷、杨梅素、槲皮素、柚皮素和山柰酚8种有效成分的分析方法。以乙腈和0.1%（v/v）甲酸水溶液为流动相进行梯度洗脱，经Dikma Diamonsil C₁₈柱分离，采用电喷雾离子源以负离子多反应监测模式进行质谱检测。结果表明，8种有效成分在线性范围内线性关系良好（r > 0.99），回收率为99.0%~102.1%，相对标准偏差为0.9%~3.3%（n=6）。该方法高效、快速、准确，为脑心清原料药浸膏及其片剂的质量标准研究提供了一定的参考。

Simultaneous determination of eight effective constituents in Naoxinqing crude drug and tablets by high performance liquid chromatography-tandem mass spectrometry

A high performance liquid chromatography-tandem mass spectrometry method (HPLC-MS/MS) was developed for the determination of eight constituents in Naoxinqing crude drug and tablets, including protocatechuate, hyperoside, kaempferol-3-O-β-D-glucopyranoside, kaempferol-3-O-β-D-galactopyranoside, myricetin, quercetin, naringenin and kaempferol. Multiple reaction monitoring (MRM) with negative electrospray ionization (ESI^-) in MS/MS was used for quantification. The eight compounds were separated on a Dikma Diamonsil C₁₈ with the mobile phases of acetonitrile and 0.1% (v/v) formic acid aqueous solution with gradient elution. The eight compounds showed good linearity in their concentration ranges with the correlation coefficients (r) better than 0.99. The recoveries were from 99.0% to 102.1%, and the relative standard deviations (RSDs) were 0.9%-3.3% (n=6). The method is accurate, sensitive and effective. It can be used for the quality control of Naoxinqing crude drug and tablets.