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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20 μL。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3.0~30.0 μg/mL(r=0.999 8)、3.978~39.78 μg/mL(r=0.999 9);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。
OBJECTIVE: To improve the quality standard for Guibi zhitong liquor. METHODS: TLC was used for the qualitative 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 20 μL. RESULTS: The TLC spots of R. angelicae, N. incisum, R. aucklandiae and M. officinalis were clear and well separated, negative control without interference. The linear range was 3.0-30.0 μg/mL for imperatorin (r=0.999 8) and 3.978-39.78 μg/mL for cinnamaldehyde (r=0.999 9); 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). CONCLUSIONS: The improved standard more effectively control the quality of the Guibi zhitong liquor.
骨痹止痛液欧前胡素桂皮醛薄层色谱法高效液相色谱法质量标准
Guibi zhitong liquorImperatorinCinnamaldehydeTLCHPLCQuality standard
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