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目的:建立一测多评法同时测定玳玳果黄酮滴丸中活性成分柚皮苷、新橙皮苷、橙皮内酯水合物及枳属苷的含量。方法:采用高效液相色谱法,使用250-4 lichrocart C18(250 mm×4.6 mm,5μm)色谱柱,流动相为乙腈(A)-0.2%醋酸水溶液(B),线性梯度洗脱(0~10 min,22%A;10~20 min,22%A→35%A;20~25 min,35%A→48%A;25~30 min,48%A→22%A),流速1.0 m L·min-1,检测波长284 nm,柱温25℃,进样量20μL。柚皮苷、新橙皮苷、橙皮内酯水合物及枳属苷的色谱峰分离度R>1.5,理论塔板数按柚皮苷计>3 000。建立测定代表性成分柚皮苷含量并以其为内参物,通过柚皮苷与新橙皮苷、橙皮内酯水合物和枳属苷的相对校正因子计算新橙皮苷、橙皮内酯水合物和枳属苷含量的一测多评法,实现多指标成分的同步测定;同时与外标法分别测定玳玳果黄酮滴丸上述4个成分含量的结果比较。结果:柚皮苷质量浓度在119.40~477.60μg·m L-1、新橙皮苷质量浓度在122.20~488.80μg·m L-1、橙皮内酯水合物质量浓度在7.62~22.86μg·m L-1、枳属苷质量浓度在3.00~21.00μg·m L-1范围内线性关系良好;柚皮苷、新橙皮苷、橙皮内酯水合物、枳属苷平均加样回收率(n=3)分别为98.67%(RSD=1.5%)、98.20%(RSD=0.50%)、101.9%(RSD=1.7%)、100.9%(RSD=0.35%);柚皮苷与新橙皮苷、橙皮内酯水合物、枳属苷的相对校正因子分别为1.153、0.434、0.893,RSD(n=6)分别为2.7%、3.1%、1.2%;外标法与一测多评法含量测定结果无显著性差异。结论:以柚皮苷为内参物,利用相对校正因子一测多评法同时测定玳玳果黄酮滴丸活性成分柚皮苷、新橙皮苷、橙皮内酯水合物与枳属苷含量的结果准确,为以中药有效部位为原料制备的中药制剂实现多指标成分群质量控制评价提供了可借鉴的方法。
OBJECTIVE: To establish a multi-evaluation method for the simultaneous determination of the content of naringin, neohesperidin, apigenol hydrate and kaempferide in toadstool flavone dropping pills. Methods: A 250-4 lichrocart C18 column (250 mm × 4.6 mm, 5 μm) was used with the mobile phase of acetonitrile (A) -0.2% acetic acid (B) and linear gradient elution (0 ~ 10 min at 22% A; 10-20 min at 22% A → 35% A; 20-25 min at 35% A → 48% A; 25-30 min at 48% A → 22% L · min-1, detection wavelength 284 nm, column temperature 25 ℃, injection volume 20μL. Naringin, neohesperidin, neotolactone hydrate and kaempferol chromatography peak separation R> 1.5, the number of theoretical plates naringin> 3000. The naringin content was determined and the relative content of naringin, neohesperidin, hesperidin and triflumina glycoside was calculated based on the content of naringin. Hydrate and flavonoids glycosides content of a multi-test method to achieve simultaneous determination of multi-index components; at the same time with the external standard method were determined Daihatsu flavonoids dropping pills content of the above four components compared results. Results: The concentration of naringin was 119.40 ~ 477.60μg · m L-1, the concentration of neohesperidin was 122.20 ~ 488.80μg · m L-1, the content of hydantoin lactone hydrate was between 7.62 ~ 22.86μg · m L-1, the calibration curve was linear over the range of 3.00 ~ 21.00 μg · m L-1. The average recoveries of naringin, neohesperidin, n = 3) were 98.67% (RSD = 1.5%), 98.20% (RSD = 0.50%), 101.9% with RSD = 1.7% and 100.9% with RSD = 0.35% (P <0.05). The relative calibration factors of triamcinolone acetonide, triamcinolone acetonide and triflumina glycoside were 1.153,0.434,0.893 and RSD (n = 6) were 2.7%, 3.1% and 1.2% No significant difference between the results of the test. Conclusion: The naringin, neohesperidin, nelumbinol hydrate and the content of trifolin were determined simultaneously with naringin as the reference material by using the relative calibration factor - The result is accurate, which provides a reference method for the quality control evaluation of multi-index component group based on the traditional Chinese medicine preparations prepared from the effective parts of traditional Chinese medicine.