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目的建立UPLC-MS/MS法同时测定康艾注射液中11种成分(毛蕊异黄酮、毛蕊异黄酮苷、人参皂苷Rg1、人参皂苷Re、芒柄花素、黄芪甲苷、人参皂苷Rf、人参皂苷Rb2、人参皂苷Rc、人参皂苷Rd、人参皂苷Rb1)的方法。方法采用正负离子切换多反应监测模式(MRM),ESI离子源;Phenomenex C18色谱柱(100 mm×3.0 mm,2.6μm)进行分离,流动相为甲醇(A)、乙腈(B)、5 mmol/L乙酸铵-0.05 mmol/L乙酸钠水溶液(C),梯度洗脱,分析时间为7.0 min。结果所测11种主要有效成分在测定浓度范围内线性关系良好,r均大于0.99;精密度、重复性和稳定性良好;平均加样回收率为95.2%~104.4%,RSD≤4.64%。4个批次康艾注射液中毛蕊异黄酮、毛蕊异黄酮苷、人参皂苷Rg1、人参皂苷Re、芒柄花素、黄芪甲苷、人参皂苷Rf、人参皂苷Rb2、人参皂苷Rc、人参皂苷Rd、人参皂苷Rb1测得量分别为0.004~0.006μg/m L、0.002~0.003μg/m L、125.75~148.00μg/m L、51.75~77.00μg/m L、0.010~0.013μg/m L、51.50~87.75μg/m L、27.83~30.73μg/m L、4.23~5.15μg/m L、8.40~13.35μg/m L、17.33~27.68μg/m L和9.03~11.00μg/m L。结论首次建立可同时测定康艾注射液的11种主要成分的UPLC-MS/MS方法,该法操作简便,灵敏度高,专属性好,分析速度快,可用于康艾注射液的质量控制。
OBJECTIVE To establish a method for simultaneous determination of eleven components in Kangai injection by UPLC-MS / MS (Ralstonia Isatis, Corydalis Granuloside, ginsenoside Rg1, ginsenoside Re, formononetin, astragaloside, ginsenoside Rf, ginsenoside Rb2 , Ginsenoside Rc, ginsenoside Rd, ginsenoside Rb1). Methods The separation was carried out on a Phenomenex C18 column (100 mm × 3.0 mm, 2.6 μm) by using positive and negative ion switching MRM (MRM) and ESI ion source. The mobile phase consisted of methanol (A), acetonitrile L ammonium acetate -0.05 mmol / L sodium acetate aqueous solution (C), gradient elution, analysis time was 7.0 min. Results The results showed that the 11 main active ingredients tested had a good linear relationship in the range of determination concentration. The average r was greater than 0.99. The precision, repeatability and stability were good. The average recoveries were 95.2% -104.4% and RSD ≤ 4.64%. 4 batches of Kangai injection calycosin, calycosin, ginsenoside Rg1, ginsenoside Re, formononetin, astragaloside, ginsenoside Rf, ginsenoside Rb2, ginsenoside Rc, ginsenoside Rd, ginseng Saponins Rb1 measured were 0.004 to 0.006 μg / mL, 0.002 to 0.003 μg / mL, 125.75 to 148.00 μg / mL, 51.75 to 77.00 μg / mL, 0.010 to 0.013 μg / mL, and 51.50 to 87.75, respectively 27.83 to 30.73 μg / m L, 4.23 to 5.15 μg / m L, 8.40 to 13.35 μg / m L, 17.33 to 27.68 μg / m L and 9.03 to 11.00 μg / m L, respectively. Conclusions The UPLC-MS / MS method for the simultaneous determination of 11 major components of Kangai injection was established for the first time. The method is simple, sensitive, specific and fast in analysis. It can be used for the quality control of Kangai injection.