牡丹花粉口含片的质量标准研究

Study on Quality Standard for Peony Pollen Buccal Tablets

目的:建立牡丹花粉口含片的质量控制方法,为其质量标准的拟定提供参考。方法:按2015年版《中国药典》(四部)薄层色谱(TLC)法对牡丹花粉口含片中的芍药苷、山柰酚、木犀草素进行定性鉴别;采用双波长-高效液相色谱(HPLC)法对牡丹花粉口含片中的芍药苷和氧化芍药苷进行定量分析[色谱柱为Agilent TC-C_(18);流动相为乙腈(A)-0.1%磷酸水溶液(B),梯度洗脱;流速为1.0 mL/min;检测波长芍药苷为230 nm、氧化芍药苷为258 nm;进样量为20μL]。结果:芍药苷、山柰酚、木犀草素的TLC鉴别结果显示,在样品图谱中,与对照品图谱相应位置上均显相同颜色的特征斑点,且阴性对照无干扰。芍药苷和氧化芍药苷的检测质量浓度分别在7.2～86.4、2.72～32.64μg/mL范围内与各自峰面积呈良好的线性关系(r≥0.999 7);平均加样回收率分别为99.12%、98.65%,RSD分别为1.54%、2.53%(n=6);精密度(n=6)、稳定性(n=8)、重复性(n=6)试验的RSD均小于3.0%。结论:该方法操作简便、重复性好,可用于牡丹花粉口含片的质量控制。

OBJECTIVE:To establish a method for quality control of Peony pollen buccal tablets,and to provide reference for the formulation of quality standard. METHODS:TLC method was used for qualitative identification of paeoniflorin,kaempferol and luteolin in Peony pollen buccal tablets according to 2015 edition of Chinese Pharmacopeia (part Ⅳ). The contents of paeoniflorin and oxypaeoniflorin in Peony pollen buccal tablets were determined by dual-wavelength HPLC method [The determination was perform on Agilent TC-C18 column with mobile phase consisted of acetonitrile (A)-0.1% phosphoric acid solution(B)with gradient elution at the flow rate of 1.0 mL/min. The detection wavelength was set at 230 nm for paeoniflorin and 258 nm for oxypaeoniflorin. Sample size was 20 μL]. RESULTS:TLC identification of paeoniflorin,kaempferol and luteolin showed that the same color characteristic spots of control chromatogram appeared in the corresponding positions of sample chromatogram without interference from negative samples. The linear range of paeoniflorin and oxypaeoniflorin were 7.2-86.4 μg/mL and 2.72-32.64 μg/mL(r≥0.999 7),respectively. The average recoveries were 99.12% and 98.65%,and RSD were 1.54% and 2.53%(n=6),respectively. RSDs of precision(n=6),stability(n=8)and reproducibility(n=6)tests were all lower than 3.0%. CONCLUSIONS:The method is simple and reproducible,and can be used for quality control of Peony pollen buccal tablets.