皮炎灵搽剂质量标准研究

Quality Standard of Piyanling Liniment

目的建立皮炎灵搽剂的质量标准。方法鉴别制剂的理化性质;采用薄层色谱(TLC)法定性鉴别制剂中的冰片;进行相对密度等相关项检查和刺激性试验。采用高效液相色谱法测定制剂中间苯二酚和水杨酸含量,色谱柱为Dikma Diamonsil C_(18)柱(150 mm×4.6 mm,5μm),流动相为甲醇-2%乙酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长为270 nm,柱温为35℃,进样量为20μL。结果制剂理化特征符合规定;冰片的TLC图斑点清晰,分离度好,阴性对照无干扰;制剂相对密度为1.113,pH为2.7,最低装量为(20.08±0.56) mL,样品细菌数≤100 cfu/mL,霉菌数≤10 cfu/mL,金黄色葡萄球菌、铜绿假单胞菌未检出; 24 h皮肤未见红肿。间苯二酚和水杨酸检测质量浓度线性范围分别为0.02～0.20 mg/mL,r=0.999 5(n=8),0.01～0.10 mg/mL,r=0.999 3(n=8);精密度、稳定性、重复性试验结果的RSD均小于2%,平均加样回收率分别为99.19%和98.16%,RSD分别为2.59%和2.12%(n=9)。结论该方法可为建立皮炎灵搽剂的质量标准提供参考。

Objective To establish the quality standard of Piyanling Liniment.Methods The physicochemical properties of Piyanling Liniment was identified.TLC methed was used for the qualitative identification of borneol in the preparation,the relative density and other related items were examined and the irritation test was carried out.HPLC method was used for the content determination of resorcinol and salicylic acid in the preparation,the chromatographic column was Dikma Diamonsil C18column(150 mm × 4.6 mm,5 μm),the mobile phase was methanol-2% acetic acid solution(gradient elution),the flow rate was 1.0 mL/min,the detection wavelength was270 nm,the column temperature was 35 ℃,and the sample size was 20 μL.Results The physicochemical properties of Piyanling Liniment were in conformity with the regulations,the TLC chromatographic spots of borneol were clear with good separation,and the negative control had no interference.The relative density of the preparation was 1.113,the pH was 2.7,the lowest loading was(20.08 ± 0.56)mL,the number of bacteria in the sample was not more than 100 cfu/mL,and the number of moulds was not more than 10 cfu/mL.Staphylococcus aureus and Pseudomonas aeruginosa were not detected.No swelling was observed in the skin within 24 h.Resorcinol showed a good linear relationship with peak area in the range of 0.02-0.20 mg/mL,r=0.999 5(n=8).Salicylic acid showed a good linear relationship with peak area in the range of 0.01-0.10 mg/mL,r=0.999 3(n=8).The RSDs of precision,stability and repeatability test results were all less than 2%.The average recovery rates of resorcinol and salicylic acid were 99.19% and 98.16%,RSDs were 2.59% and 2.12%(n=9).Conclusion This method can provide a reference for establishing the quality standard of Piyanling Liniment.