[关键词]
[摘要]
目的 建立一种快速、准确和实用的HPLC方法,用于同时测定杞菊地黄口服液中5-羟甲基糠醛(5-HMF)、莫诺苷、绿原酸、隐绿原酸、马钱苷、芍药苷、毛蕊花糖苷、木犀草苷、异绿原酸B、异绿原酸A、异绿原酸C、丹皮酚的含量。方法 采用YMC ODS柱(250 mm×4.6 mm,5 μm),柱温35℃,以0.1%甲酸水溶液-乙腈为流动相进行梯度洗脱,体积流量为1.0 mL/min,检测波长为254、325 nm,进样量10 μL。结果 5-HMF、莫诺苷、绿原酸、隐绿原酸、马钱苷、芍药苷、毛蕊花糖苷、木犀草苷、异绿原酸B、异绿原酸A、异绿原酸C、丹皮酚进样量在0.08~1.60、0.12~2.40、0.09~1.80、0.06~1.20、0.10~2.00、0.30~6.00、0.01~0.20、0.01~0.20、0.01~0.20、0.005~0.10、0.005~0.10、0.01~0.20 μg与峰面积呈良好的线性关系,精密度、重复性、稳定性均良好,RSD均小于3.5%,加样回收率均在96%~103%,RSD分别为2.13%、3.45%、2.86%、2.59%、3.15%、3.49%、2.19%、3.25%、2.37%、2.53%、2.91%、3.35%,测定5批样品中各成分含量稳定,所测12种成分质量浓度分别为98.56~102.56、204.28~212.10、18.53~18.89、1.95~2.05、12.31~12.54、87.01~87.12、5.35~5.43、16.08~16.15、8.69~8.72、8.89~8.95、5.12~5.19、1.87~1.94 μg/mL。结论 本方法可以同时测定杞菊地黄口服液中5-HMF、莫诺苷、绿原酸、隐绿原酸、马钱苷、芍药苷、毛蕊花糖苷、木犀草苷、异绿原酸B、异绿原酸A、异绿原酸C、丹皮酚的含量,适用于杞菊地黄口服液的质量控制。
[Key word]
[Abstract]
Objective To establish a rapid, accurate, and practical HPLC method for simultaneous determination the content in Qiju Dihuang Oral Liquid (QDOL) of 5-HMF, morroniside, chlorogenic acid, cryptochlorogenic acid, loganin, paeoniflorin, verbascoside, luteoloside, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, and paeonol. Methods YMC ODS column (250 mm×4.6 mm, 5 μm) was used, column temperature was set at 35℃, gradient elution with 0.1% formic acid aqueous solution-acetonitrile was used as mobile phase, flow rate was 1.0 mL/min, detection wavelength was 254 and 325 nm. The injection volume was 10 μL. Results The injection amount of 5-HMF, morroniside, chlorogenic acid, cryptochlorogenic acid, loganin, paeoniflorin, verbascoside, luteoloside, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, paeonol injection quality at 0.08-1.60, 0.12-2.40, 0.09-1.80, 0.06-1.20, 0.10-2.00, 0.30-6.00, 0.01-0.20, 0.01-0.20, 0.01-0.20, 0.005-0.10, 0.005-0.10, and 0.01-0.20 μg showed a good linear relationship with peak area, with good precision, repeatability and stability. The recovery rates of the samples were between 96% and 103%, the RSD was 2.13%, 3.45%, 2.86%, 2.59%, 3.15%, 3.49%, 2.19%, 3.25%, 2.37%, 2.53%, 2.91%, and 3.35%, respectively. The content of each component of the five batches of samples was stable, and the mass concentrations range of the 12 components tested were 98.56-102.56, 204.28-212.10, 18.53-18.89, 1.95-2.05, 12.31-12.54, 87.01-87.12, 5.35-5.43, 16.08-16.15, 8.69-8.72, 8.89-8.95, 5.12-5.19, and 1.87-1.94 μg/mL. Conclusion The method simltaneosly determines the content of 5-HMF, morroniside, chlorogenic acid, cryptochlorogenic acid, loganin, paeoniflorin, verbascoside, luteoloside, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, and paeonol in QDOL, which is suitable for the quality control of QDOL.
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[基金项目]
江苏省重点研发计划——社会发展项目(BE2016626)