辛夷配方颗粒UPLC指纹图谱及含量测定研究

Study on Establishment of UPLC Fingerprint and Content Determination of Magnoliae Flos Formula Granules

目的建立辛夷配方颗粒超高效液相色谱(UPLC)指纹图谱,并测定主要有效成分木兰脂素和木兰花碱含量,为辛夷配方颗粒的质量控制提供参考。方法采用YMC Triart C18色谱柱(2.1 mm×100 mm,1.9μm),以乙腈-0.1%磷酸溶液为流动相,梯度洗脱,流速0.3 mL/min,检测波长230 nm,建立辛夷配方颗粒指纹图谱,并采用超高效液相色谱-质谱联用(UPLC-MS)技术对共有指纹峰进行指认,同时测定辛夷配方颗粒中木兰脂素和木兰花碱的含量。结果辛夷配方颗粒指纹图谱共标定7个共有峰,指认了其中4个峰,分别为木兰脂素、木兰花碱、松脂素二甲醚和表木兰脂素B;不同批次辛夷配方颗粒指纹图谱与对照指纹图谱的相似度为0.965~0.997;10批辛夷配方颗粒木兰脂素含量为18.65~27.87 mg/g,木兰花碱含量为21.20~32.97 mg/g,不同批次间含量存在一定差异。结论本研究建立的UPLC指纹图谱及含量测定方法准确、快捷、专属性良好,可以为辛夷配方颗粒的质量控制提供参考。

Objective To establish the ultra high performance liquid chromatography(UPLC)fingerprints;To determine the contents of magnolin and magnoflorine;To provide a reference for the quality control of Magnoliae Flos(Xinyi)Formula Granules.Methods The chromatographic column was YMC Triart C18(2.1 mm×100 mm,1.9μm).The mobile phase was acetonitrile-0.1%phosphoric acid solution with gradient elution.The flow rate was 0.3 mL/min;the detection wavelength was 230 nm.The fingerprint of Xinyi Formula Granuleswas established and the common fingerprint peaks were identified by ultra high performance liquid chromatography-mass spectrometry(UPLC-MS).Meanwhile,the contents of magnolin and magnoflorine were determined.Results Seven common peaks were calibrated in the fingerprint of Xinyi Formula Granules.Four peaks were identified as magnolin,magnoflorine,pinoresin dimethyl ether and epimagnolia B;the similarity between the fingerprints of different batches of Xinyi Formula Granules and the control fingerprint was between 0.965–0.997.The content of magnolin in 10 batches of Xinyi Formula Granules ranged from 18.65 mg/g to 27.87 mg/g.The content of magnoflorine ranged from 21.20 mg/g to 32.97 mg/g.There were some differences in content between different batches.Conclusion The UPLC fingerprint and content determination method established in this study are accurate,fast and specific,which can provide a reference for the quality control of Xinyi Formula Granules.