摘要
目的：建立测定中药注射液中5-羟甲基糠醛含量的高效液相色谱-串联质谱联用分析方法。方法：采用Zorbax SB-C18（150 mm×2.1 mm,5μm）色谱柱;流动相为甲醇-0.1%甲酸溶液（20∶80）;流速为0.20 mL·min^-1;柱温为室温;采用电喷雾离子源（ESI）,多反应监测扫描模式（MRM）进行定量分析。结果：峰面积Y与浓度X在0.05～20.0μg·mL^-1范围内线性关系良好（r=0.9993）,检测限为10.0 ng·mL^-1,平均加样回收率（n=9）为99.2%,精密度试验的RSD为1.9%,重复性试验的RSD为1.8%。结论：本研究建立的分析方法灵敏,快捷、准确,重复性好,适用于中药注射液中5-羟甲基糠醛的含量分析及质量控制研究。
Objective：To establish a sensitive and rapid HPLC-MS/MS method for the determination of 5-hydroxymethyl furfural in Chinese traditional medicine injection.Methods：The HPLC separation was performed on Zorbax SB-C18（150 mm × 2.1 mm,5 μm）with methanol added 0.1% formic acid solvent mixture solution（20∶ 80） as the mobile phase,the flow rate was 0.2 mL·min^-1,column temperature was room temperature.Electrospray ionization（ESI）source was used.Quantization was performed by using selected multiple reaction monitoring（MRM）mode.Results： The results showed the linear range of 5-hydroxymethyl furfural was 0.05-20.0 μg·mL^-1（r=0.9993）,the limit of quantization was 10.0 ng·mL^-1,the average recovery rate（n=9）was 99.2%,the RSD（n=5）of precision test and reproducibility test were 1.9% and 1.8%.Conclusion： The method is sensitive,rapid and accurate with good repeatability,which can be used for determination of the content and the quality control of 5-hydroxymethyl furfural in Chinese traditional medicine injection.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2010年第7期1195-1198,共4页
Chinese Journal of Pharmaceutical Analysis
