骨痹止痛液的质量标准提高研究

摘要

OBJECTIVE:To improve the quality standard for Guibi zhitong liquor. METHODS:TLC was used for the qualita-tive identification of Radix angelicae,Notopterygium incisum,Radix aucklandiae and Magnolia officinalis in the preparation;HPLC was used for the contents determination of imperatorin and cinnamaldehyde:the column was Waters Symmetry Shield RP-C18 with mobile phase of methanol-water for imperatorin(60:40,V/V)and methanol-water for cinnamaldehyde(35:65,V/V)at a flow rate of 1.0 mL/min,detection wavelength was 254 nm for imperatorin and 290 nm for cinnamaldehyde,column temperature was 25℃,and the injection volume was 20μL. RESULTS:The TLC spots of R. angelicae,N. incisum,R. aucklandiae and M. of-ficinalis were clear and well separated,negative control without interference. The linear range was 3.0-30.0 μg/mL for imperatorin (r=0.9998)and 3.978-39.78 μg/mL for cinnamaldehyde(r=0.9999);RSDs of precision,stability and reproducibility tests were lower than 2.0%;recoveries were 96.94%-102.64%(RSD=2.37%,n=6)and 96.78%-99.53%(RSD=1.00%,n=6). CONCLU-SIONS:The improved standard more effectively control the quality of the Guibi zhitong liquor.%目的:提高骨痹止痛液的质量标准.方法:采用薄层色谱法(TLC)对制剂中独活、羌活、木香、厚朴进行定性鉴别;采用高效液相色谱法测定制剂中欧前胡素、桂皮醛的含量:色谱柱为Waters Symmetry Shield RP-C18,流动相为甲醇-水(60:40,V/V,欧前胡素)、甲醇-水(35:65,V/V,桂皮醛),流速为1.0 mL/min,检测波长为254 nm(欧前胡素)、290 nm(桂皮醛),柱温为25℃,进样量为20μL.结果:独活、羌活、木香、厚朴的TLC图斑点清晰,分离度好,阴性对照无干扰.欧前胡素、桂皮醛检测质量浓度线性范围分别为3.0~30.0μg/mL(r=0.9998)、3.978~39.78μg/mL(r=0.9999);精密度、稳定性、重复性试验的RSD<2.0%;加样回收率分别为96.94%~102.64%(RSD=2.37%,n=6)、96.78%~99.53%(RSD=1.00%,n=6).结论:提高的标准能更加有效地控制骨痹止痛液的质量.