摘要
目的:建立测定7-(2-二甲氨基乙氧基)黄酮(wx-03)原料药中主药含量的方法。方法:采用高效液相色谱串联质谱(HPLC-MS/MS)法。色谱柱为AgilentC18,流动相为5mmol·L-1乙酸铵缓冲液(pH3.5)-甲醇-乙腈(10:40:50),流速为0.6mL·min-1,柱温为30℃;离子源为电喷雾电离源,正离子模式,扫描方式为多反应监测,用于定量分析的离子对为m/z309.8→m/z265.2,扫描时间为200ms。结果:wx-03的检测浓度线性范围为10～100mg·L-1(r=0.9995),平均回收率为99.9%,RSD=0.27%,最低检测限为0.2mg·L-1。结论:该法适用于黄酮类化合物wx-03原料药的含量测定。
OBJECTIVE：To establish the method for the content determination of 7-（2-dimethylamino ethoxy） flavone（wx-03）in its crude drug.METHODS：HPLC method was adopted.The determination was performed on Agilent C 18 column with mobile phase consisted of 5 mmol·L-1 ammonium acetate buffer solution（pH adjusted to 3.5）-methanol-acetonitrile（10：40：50）at the flow rate of 0.6 mL·min-1 with column temperature of 30 ℃.HPLC-MS/MS was operated under the selective reaction monitoring mode using the electrospray ionization technique in positive mode.The ion pair for quantitative analysis was m/z 309.8→m/z 265.2,and scanning time was 200 ms.RESULTS：The linear range of wx-03 was 10～100 mg·L-1（r=0.999 5）with an average recovery of 99.9%（RSD=0.27%）.Limit of detection was 0.2 mg·L-1.CONCLUSION：The method is suitable for the content determination of wx-03 in crude drug.
出处
《中国药房》
CAS
CSCD
2012年第45期4299-4300,共2页
China Pharmacy
