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

摘要

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越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。%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. Mul-tiple reaction monitoring( MRM)with negative electrospray ionization( ESI-)in MS/MS was used for quantification. The eight compounds were separated on a Dikma Diamonsil C 18 with the mobile phases of acetonitrile and 0. 1%( v/v)formic acid aqueous solution with gradient elu-tion. The eight compounds showed good linearity in their concentration ranges with the correla-tion coefficients( r)better than 0. 99. The recoveries were from 99. 0% to 102. 1%,and the rel-ative 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.