宣肺达郁颗粒质量标准研究

Study on Quality Standard of Xuanfei Dayu Granules

目的建立宣肺达郁颗粒的质量标准。方法采用薄层色谱(TLC)法对制剂中陈皮、白芍、百合、干姜进行定性鉴别;采用高效液相色谱(HPLC)法同时测定制剂中苦杏仁苷、芍药苷、甘草苷、桂皮醛、橙皮苷的含量,色谱柱为Agilent 5 TC-C18柱(150 mm×4.6 mm,5μm),流动相为甲醇-0.2%乙酸水溶液(梯度洗脱),流速为1.0 mL/min,检测波长为220 nm,柱温为30℃,进样量为15μL。结果陈皮、白芍、百合、干姜的TLC图斑点清晰,分离度好,且阴性对照无干扰。苦杏仁苷、芍药苷、甘草苷、桂皮醛、橙皮苷质量浓度分别在1.0640~19.1520μg/mL、0.8200~14.7600μg/mL、0.1380~2.4840μg/mL、0.0005~0.0090μg/mL、0.4320~7.7760μg/mL范围内与峰面积线性关系良好(R^(2)≥0.9992);精密度、稳定性、重复性试验结果的RSD均小于3.0%;平均加样回收率分别为97.26%,102.46%,95.63%,98.61%,97.73%;RSD分别为1.69%,3.56%,2.19%,2.64%,0.99%(n=6)。结论该研究中所建立的标准操作简便,专属性强,结果准确可靠,可用于宣肺达郁颗粒的质量控制。

Objective To establish the quality standard of Xuanfei Dayu Granules.Methods Citri Reticulatae Pericarpium,Paeoniae Radix Alba,Lilii Bulbus,Zingiberis Rhizoma in the preparation were identified qualitatively by the thin-layer chromatography(TLC)method,the contents of amygdalin,paeoniflorin,liquiritin,cinnamaldehyde and hesperidin in the preparation were determined simultaneously by the high-performance liquid chromatography(HPLC)method.The chromatographic column was Agilent 5 TC-C18 column(150 mm×4.6 mm,5μm),the mobile phase was methanol-0.2%acetic acid aqueous solution(gradient elution),the flow rate was 1.0 mL/min,the detection wavelength was 220 nm,the column temperature was 30℃,and the injection volume was 15μL.Results The TLC chromatograms of Citri Reticulatae Pericarpium,Paeoniae Radix Alba,Lilii Bulbus and Zingiberis Rhizoma showed clear spots,good resolution,and there was no interference from the negative reference.The linear ranges of amygdalin,paeoniflorin,liquiritin,cinnamaldehyde and hesperidin were 1.0640-19.1520μg/mL,0.8200-14.7600μg/mL,0.1380-2.4840μg/mL,0.0005-0.0090μg/mL,0.4320-7.7760μg/mL(R^(2)↓0.9992)respectively.The RSDs of precision,stability and repeatability tests were all lower than 3.0%.The average recovery rates of the above five components were 97.26%,102.46%,95.63%,98.61%,97.73%with RSDs of 1.69%,3.56%,2.19%,2.64%,0.99%(n=6),respectively.Conclusion The established standard is simple,specific,accurate and reliable,which can be used for the quality control of Xuanfei Dayu Granules.