定痛膏的质量标准提高研究

Study on the Improvement of Quality Standard of Dingtong Ointments(定痛膏)

目的:完善和提高定痛膏的质量标准。方法:采用薄层色谱法(TLC)对定痛膏中木香、大黄、黄连进行定性鉴别。采用高效液相色谱法对定痛膏中有毒成分次乌头碱进行限量检测:色谱柱为Benetnach C18,以乙腈-四氢呋喃(25∶15,V/V)为流动相A,以0.1 mol/L醋酸铵溶液为流动相B,流速为0.8 m L/min,检测波长为235 nm,柱温为30℃,进样体积为10μL。结果:木香、大黄、黄柏的TLC图斑点清晰,分离度好,阴性对照均无干扰。次乌头碱检测限为1.25×10-2μg,定量限为3.75×10-2μg,HPLC法所测3批定痛膏中次乌头碱含量均未超出规定限度。结论:完善和提高的标准有利于定痛膏的质量控制。

Objective： To optimize and improve the quality standards of Dingtong Ointments （定痛膏）. Meth- ods： TLC was used for qualitative identification of muxiang （Radix Aucklandiae）, dahuang （Rheum officinale） and huanglian （Cortex phellodendri）. HPLC was used for the content determination of Hypaconitine. Column was Benetnach C18 with mobile phase A of Acetonitrile/tetrahydrofurann （25：15, V/V） and mobile phase B of ammoni- um acetate （0.1 mol/L）at a flow rate of 0.8 mL/min, the detection wavelength was 235 nm, the column tempera- ture was 30 ℃, and the injection volume was 10 μL. Results： The TLC of Radix Aucklandiae, Rheum officinale and Cortex phellodendri showed clear spots and good separation, non-interference in negative control. The detection limit and quantization limit were 1.25×10-2 μg and 3.75×10-2 μg. The hypaconitine in Dingtong Ointments of three batches were all within specified ranges. Conclusions： The optimized and improved method is helpful for the quality eontrol of Dingtong Ointments.