蒲地金黄贴质量标准的研究

The quality standard of Pudi Jinhuang Paste

目的确定蒲地金黄贴定性、定量检测方法,建立其质量标准。方法采用薄层色谱法鉴别黄芩、栀子;采用显微鉴定法鉴定大黄、黄柏、侧柏叶;应用高效液相色谱法测定盐酸小檗碱的含量,选用Agilent ZORBAX-SB-C18色谱柱,以0.1%磷酸溶液-乙腈(50∶50)(每100 ml加十二烷基磺酸钠0.1 g)为流动相,流速为1.0 ml/min,进样量5μl,检测波长为265 nm,柱温30℃。结果薄层色谱法检测黄芩、栀子图谱特征斑点清晰,阴性无干扰,专属性强;大黄、黄柏和侧柏叶的显微特征均明显;黄柏中盐酸小檗碱进样量在12.5~498.4 ng内与峰面积呈良好的线性关系(r=1.0000),平均加样回收率为99.7%(RSD=1.69%,n=9)。结论该方法专属性强、简便,可作为蒲地金黄贴的质量控制方法。

Objective To determine the qualitative and quantitative methods for the determination of Pudi Jinhuang Paste,so as to establish its quality standard.Methods The scutellaria and gardenia jasminoides were identified by thin-layer chromatography,and the rhubarb,phellodendron chinense and platycladus orientalis leaves were identified by microscope.The content of berberine hydrochloride was determined by UPLC using an Agilent ZORBAX SB-C18 column with 0.1%phosphoric acid solution-acetonitrile(50∶50)(0.1 g of sodium dodecyl sulfate per 100 ml)as the mobile phase.The flow rate was 1.0 ml/min,the injection volume was 5μl.The detection wavelength was 265 nm,and the column temperature was 30℃.Results The chromatogram for thin-layer chromatography detecting scutellaria and gardenia jasminoides showed clear spots,with strong specificity and no interference of negative samples.The microscopic characteristics of rhubarb,phellodendron chinense and platycladus orientalis leaves were all obvious.The berberine hydrochloride in phellodendron chinense showed good linearity(r=1.0000)with the peak area with an injection volume range of 12.5-498.4 ng,and the average spiked recovery was 99.7%(RSD=1.69%,n=9).Conclusion This method is specific and simple and can be used as a quality control method for Pudi Jinhuang P aste.