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作 者:孙熠[1] 耿婷[1] 单鸣秋[1] 张丽[1] 丁安伟[1,2]
机构地区:[1]南京中医药大学,南京210046 [2]江苏省方剂研究重点实验室,南京210046
出 处:《中国实验方剂学杂志》2011年第5期52-55,共4页Chinese Journal of Experimental Traditional Medical Formulae
基 金:国家科技重大专项课题:创新药物研究开发-候选药物研究(2009ZX09103-339)
摘 要:目的:建立荆芥内酯的含量测定方法和有关物质的分析方法。方法:指定以Waters XTerra MS C18色谱柱进行有关物质分析,指定以Kromasil C18色谱柱进行含量测定,以甲醇-水(45∶55)为流动相(氢氧化钠调pH至10.0),流速为0.8mL·min-1,柱温30℃,检测波长216 nm。结果:荆芥内酯与有关物质及各降解成分完全分离;荆芥内酯质量浓度在0.012 6~0.403 6 g·L-1与峰面积呈良好线性关系,r=0.999 9;最低检测限0.25μg,最小定量限为0.63μg;平均回收率100.04%,RSD为1.40%。结论:该方法操作简便、快速、准确,灵敏度高,可用于荆芥内酯含量及有关物质的测定。Objective:To establish an HPLC method for the determination of content and related substances in schizonepetin. Method:Two stability columns based on silica gel were used respectively( Waters XTerra MS C18 column for related substances analysis; And Kromasil C18 column for content determination). The mobile phase con- sisted of methanol-water(45:55 ), and when analyzing substances destroyed by alkali, the pH value of the mobile phase should be adjusted to 10.0 by sodium hydroxide. Both of the two columns were maintained at a constant tem- perature of about 30 ℃. The flow rate was 0.8 mL per minute. The UV detection wavelength was set at 216 nm. Resuit:Related substances and degraded substances were completely separated from schizonepetin. The linear range of determination was 0. 012 6-0. 403 6 g.L-1 with the correlation coefficient of 0. 999 9. The LOD was 0.25 μg,and the LOQ was 0.63 μg. The average recovery was 100.04% , RSD 1.40%. Conclusion: The method is simple, rapid, accurate, and sensitive and it is suitable for the determination of the content and related substances in schizonepetin.
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