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目的:提高复方守宫散的质量标准。方法:采用显微鉴别法对制剂中壁虎、梅花进行显微鉴别;采用薄层色谱法(TLC)对制剂中制何首乌进行定性鉴别;采用高效液相色谱法(HPLC)测定制剂中2,3,5,4′ -四羟基二苯乙烯-2-O-β-D-葡萄糖苷(简称“二苯乙烯苷”)的含量:色谱柱为Agilent Zorbax Eclipse XDB-C18,流动相为乙腈-水(19 ∶ 81,V/V),流速为1.0 mL/min,检测波长为320 nm,柱温为25 ℃,进样量为10 μL。结果:壁虎的皮肤碎片和鳞片、梅花的花粉粒显微特征明显,阴性对照无干扰。制何首乌的TLC图斑点清晰,分离度好,阴性对照无干扰。二苯乙烯苷检测质量浓度线性范围为23~368 μg/mL(r=0.999 9);精密度、稳定性、重复性试验的RSD<1.0%;加样回收率为98.69%~101.61%(RSD=0.94%,n=9)。结论:提高的标准能更加有效地控制复方守宫散的质量。
OBJECTIVE: To improve the quality standard of Compound shougong powder. METHODS: Gekko japonicas and Armeniaca mume were identified by microscopic identification. TLC method was adopted to identify processed Fallopia multiflora qualitatively. The content of 2,3,5,4-tetrahydroxystilbene-2-O-β-D-glucoside (stilbene glycoside) was determined by HPLC. The determination was performed on Agilent Zorbax Eclipse XDB-C18 column with mobile phase consisted of acetonitrile-water (19 ∶ 81,V/V) at the flow rate of 1.0 mL/min. The detection wavelength was set at 320 nm, and column temperature was 25 ℃. The sample size was 10 μL. RESULTS: Microscopic characteristics of skin fragments and scales of G. japonicas and the pollen grains of A. mume were significant without interference from negative control. TLC spots of F. multiflora were clear and well-separated without interference from negative control. The linear range of stilbene glucoside were 23-368 μg/mL (r=0.999 9). RSDs of precision, stability and reproducibility tests were all lower than 1.0%. The recoveries ranged 98.69%-101.61% (RSD=0.94%,n=9). CONCLUSIONS: Improved standard can effectively control the quality of Compound shougong powder.
复方守宫散显微鉴别法薄层色谱法含量测定高效液相色谱法
Compound shougong powderMicroscopy identification methodTLCContent determinationHPLC
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