满山香片的质量标准提高研究

Study on Improving the Quality Standards of Manshanxiang Tablet

目的:完善和提高满山香片的质量标准。方法:采用薄层色谱法对制剂中满山香药材、山柰素和槲皮素进行薄层定性鉴别;采用高效液相色谱法测定满山香片中山柰素的含量,色谱柱为YMC-Pack ODS-A C18柱(250 mm×4.6 mm,5μm),流动相为甲醇-0.2%磷酸溶液(V∶V=47∶53),流速为1.0 ml/min,检测波长为365 nm(山柰素),进样量为10μl。结果:山柰素和槲皮素的薄层色谱图斑点清晰,分离度好,阴性对照无干扰;山柰素检测进样量在0.041 4~0.828 4μg范围内线性关系良好(r=0.999 8),精密度、稳定性和重复性试验的RSD均<2.0%,加样回收率为95.50%~100.37%(RSD=1.80%,n=6)。结论:满山香片中满山香药材、山柰素和槲皮素的薄层色谱鉴别分离度好、专属性强;采用高效液相色谱法测定方中山柰素含量,操作方便,方法准确,重现性好,能更加有效地控制满山香片的质量。

OBJECTIVE： To perfect and improve the quality standards of Manshanxiang tablet. METHODS： Thin layer chromatography（ TLC） was adopted to conduct thin layer qualitative identification on Manshanxiang,kaempf-eride and quercetin; and high performance liquid chromatography（ HPLC） was used for determining the content kaempf-eride in Manshanxiang tablet,the chromatographic column was YMC-Pack ODS-A C18（ 250 mm ×4. 6 mm,5 μm）,with mobile phase of methyl alcohol-0. 2% of phosphoric acid solution（ V ∶ V = 47 ∶ 53） and flow velocity of 1. 0 ml/min,the detected wavelength was 365 nm（ kaempf-eride）,and sample size was 10 μl. RESULTS： Spots of TLC of kaempf-eride and quercetin were clear,with well separation degree and no interference on negative control; the sample size of kaempferide ranged from 0. 041 4-0. 828 4 μg,with well linear relation（ r = 0. 999 8）,all the RSD of precision,stability and repetitive testing were 2. 0%,the sample recovery rate was 95. 50%-100. 37%（ RSD = 1. 80%,n = 6）. CONCLUSIONS：Manshanxiang,kaempf-eride and quercetin of Manshanxiang tablet have well separation degree and strong specificity in TLC; HPLC is convenient for operation,accurate and with well reproducibility in determining the content of kaempferide,which can improve the quality of Manshanxiang tablet more effectively.