目的 建立HPLC-MS/MS同時(shí)測(cè)定同濟(jì)2號(hào)顆粒中5個(gè)主要活性成分黃芪甲苷、綠原酸、人參皂苷Rg₁、人參皂苷Rb₁及三七皂苷R₁的方法。方法 以水(0.1%甲酸)-乙腈(0.1%甲酸)為流動(dòng)相,梯度洗脫,體積流量為0.4 mL/min。YMC-Pack Pro C₈色譜柱分離,采用電噴霧離子源(ESI源),負(fù)離子模式,以選擇性離子監(jiān)測(cè)模式(SIM)進(jìn)行測(cè)定。監(jiān)測(cè)離子分別是m/z 829(黃芪甲苷)、m/z 353(綠原酸)、m/z 845(人參皂苷Rg₁)、m/z 1 108(人參皂苷Rb₁)、m/z 932(三七皂苷R₁)。結(jié)果 黃芪甲苷、綠原酸、人參皂苷Rg₁、人參皂苷Rb₁和三七皂苷R₁分別在0.075～2.4、0.95～30.3、1.71～54.72、1.12～35.92、0.45～14.28 μg/mL與峰面積呈良好線性關(guān)系。結(jié)論 該方法專(zhuān)屬性好,靈敏度高,準(zhǔn)確快捷,適用于同濟(jì)2號(hào)顆粒的快速檢測(cè),為該藥的質(zhì)量標(biāo)準(zhǔn)提供依據(jù)。

Objective To establish an LC-MS/MS method for simultaneous determination of five compounds (astragaloside IV, chlorogenic acid, ginsenosides Rg₁, Rb₁, and notoginsenoside R₁) in Tongji No. 2 granules. Methods The chromatographic separation was carried out on a YMC-Pack Pro C₈ column (150 mm × 4.6 mm, 5 μm) eluted in a gradient program. The mobile phase consisted of water containing 0.1% formic acid-acetonitrile containing 0.1% formic acid. The mass spectra were obtained by Agilent QQQ triple quad mass spectrometer with electrospray ionization source in negative ion mode. Monitoring ions are m/z 829 (astragaloside IV), m/z 353 (chlorogenic acid), m/z 845 (ginsenosides Rg₁), m/z 1 108 (ginsenosides Rb₁), and m/z 932 (notoginsenoside R₁). Results The linear ranges for astragaloside IV, chlorogenic acid, ginsenosides Rg₁, ginsenosides Rb₁, and notoginsenoside R₁ were 0.075 - 2.4, 0.95 - 30.3, 1.71 - 54.72, 1.12 - 35.92, and 0.45 - 14.28 μg/mL. Conclusion The established method is convenient, sensitive, and accurate. It can be used for the determination of the contents of the main active ingredients in Tongji No. 2 granules for quality control.

上海市中西醫(yī)結(jié)合重點(diǎn)病種建設(shè)項(xiàng)目(zxbz2012-15)