绵马贯众配方颗粒的HPLC指纹图谱研究

Study on HPLC Fingerprint of Dryopteridis Crassirhizomatis Rhizoma Dispensing Granules

关键词:  绵马贯众  配方颗粒  指纹图谱  液质联用

Key words:  Dryopteridis Crassirhizomatis Rhizoma  dispensing granules  fingerprint  LC-MS

摘要:

目的 建立绵马贯众配方颗粒的HPLC指纹图谱。方法 采用HPLC，色谱柱以C₁₈为填充剂，乙腈-1%醋酸溶液为流动相，流速为1.0 mL·min^-1进行梯度洗脱，检测波长为330 nm；采用液质联用技术（LC-MS）获得特征峰的分子量和分子离子碎片，结合对照品和文献比对等方法进行特征峰结构指认。结果 绵马贯众配方颗粒的指纹图谱呈现12个共有峰，7个共有峰进行了指认，分别为新绿原酸、绿原酸、隐绿原酸、4β-羧甲基-（–）-表儿茶素、圣草次苷、3-甲基丁酰基间苯三酚-4，6-二-C-葡萄糖苷、1-甲基-3-丁酰基间苯三酚。结论 建立了绵马贯众配方颗粒的HPLC指纹图谱，方法重复性、稳定性好，可用于绵马贯众配方颗粒的生产全过程的质量控制。

Abstract:

OBJECTIVE To establish HPLC fingerprint of Dryopteridis Crassirhizomatis Rhizoma dispensing granules. METHODS A gradient elution method with a flow rate of 1.0 mL·min^-1 and a detection wavelength of 330 nm was developed on a HPLC column using C₁₈ as a filler and acetonitrile-1% acetic acid as a mobile phase. Liquid chromatography-mass spectrometry(LC-MS) was used to obtain the molecular weight and molecular ion fragments of the characteristic peaks, and the characteristic peak structure was identified by combining reference materials and literature comparison methods. RESULTS The fingerprint consisted of 12 common peaks, and 7 common peaks were identified, which were neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, 4β-car-boxymeth-yl-(–)-epicatchin, eriocitrin, 3-methylbutyryl-phloroglucinol- 4,6-di-C-glucoside, 1-methyl-3-butyryl-phloroglucinol. CONCLUSION The HPLC fingerprint of Dryopteridis Crassirhizomatis Rhizoma dispensing granules. The method displays good stability and repeatability which is suitable for the quality evaluation of Dryopteridis Crassirhizomatis Rhizoma dispensing granules.