祛湿止痒洗剂的定性定量方法研究

目的：建立祛湿止痒洗剂的定性定量方法。方法：采用薄层色谱法对祛湿止痒洗剂中苦参、黄柏、荆芥、防风、蛇床子进行定性鉴别。采用高效液相色谱法对祛湿止痒洗剂中黄柏的主要成分黄柏碱和小檗碱进行含量测定；色谱条件：采用C₁₈色谱柱（250 mm×4.6 mm，5 μm），以乙腈-0.1%磷酸溶液为流动相，梯度洗脱，流速为1.0 mL·min^-1，检测波长为284 nm（盐酸黄柏碱，出峰时间为9 min）、265 nm（盐酸小檗碱，出峰时间为34.5 min），柱温为30℃。结果：薄层色谱中，斑点清晰，阴性对照无干扰。盐酸黄柏碱的质量浓度在80~480 μg·mL^-1（r=0.999 9），盐酸小檗碱的质量浓度在27.5~165 μg·mL^-1（r=0.999 8）范围内线性关系良好；盐酸黄柏碱平均加样回收率（n=3）分别为99.2%（RSD=0.62%）、98.9%（RSD=0.49%）、99.2%（RSD=0.51%），盐酸小檗碱平均加样回收率（n=3）分别为99.3%（RSD=0.64%）、99.3%（RSD=0.4%）、99.0%（RSD=0.26%）；3批样品中盐酸黄柏碱的含量分别为1.369、1.302、1.421 mg·mL^-1，盐酸小檗碱的含量分别为0.176、0.171、0.182 mg·mL^-1。结论：本试验所用方法可用于控制祛湿止痒洗剂的质量。

Objective: To establish a method for qualitative and quantitative analysis of Qushizhiyang lotion. Methods: Sophorae Flavescentis Radix,Phellodendri Chinensis Cortex,Schizonepetae Herba,Saposhnikoviae Radix and Cnidii Fructus were identified by TLC.Phellodendrine hydrochloride and berberine hydrochloride in Qushizhiyang lotion were determined by HPLC.The chromatographic conditions were as follows:column:C₁₈(250 mm×4.6 mm,5 μm); mobile phase:acetonitrile(A)-0.1% phosphoric acid(B)with gradient elution at the flow rate of 1.0 mL·min^-1;detection wavelengths:284 nm for phellodendrine hydrochloride eluted at 9 min and 265 nm for berberine hydrochloride eluted at 34.5 min;column temperature:30℃. Results: The TLC spots were clear without interference from negative sample.The linear ranges of phellodendrine hydrochloride and berberine hydrochloride were 80-480 μg·mL^-1(r=0.999 9)and 27.5-165 μg·mL^-1(r=0.999 8),respectively.The average recoveries(n=3)of phellodendrine hydrochloride were 99.2%(RSD=0.62%),98.9%(RSD=0.49%)and 99.2%(RSD=0.51%),and the average recoveries(n=3)of berberine hydrochloride were 99.3%(RSD=0.64%),99.3%(RSD=0.4%)and 99. 0%(RSD=0.26%).The contents of phellodendrine hydrochloride in 3 samples were 1.369,1.302 and 1.421 mg·mL^-1,respectively,and the contents of berberine hydrochloride in 3 samples were 0.176,0.171 and 0.182 mg·mL^-1,respectively. Conclusion: The method could be used for control quality of Qushizhiyang lotion.

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