高效液相色谱-示差折光检测法测定磺丁基醚-β-环糊精的含量  

Determination of sulfobutyl ether β-cyclodextrin by high performance liquid chromatography coupled with refractive index detector

作　　者：李闻新 部实 张余 刘丹[1] 张福林[1] LI Wen-xin;BU Shi;ZHANG Yu;LIU Dan;ZHANG Fu-lin(Department of Pharmacy,the Second Hospital of Tangshan City,Tangshan 063000,China)

机构地区：[1]唐山市第二医院药剂科,河北唐山063000

出　　处：《实用药物与临床》2019年第1期56-59,共4页Practical Pharmacy and Clinical Remedies

基　　金：唐山市科技计划自筹经费项目(17130236a)

摘　　要：目的建立辅料SBE_7-β-CD的含量测定方法。方法采用高效液相凝胶色谱法。Phenomenex PolySep-GFC-P3000凝胶柱(7. 8 mm×30 cm),柱温35℃;示差折光检测器,检测温度35℃;流动相:乙腈-0. 1 mol/L硝酸钾水溶液(35∶65),进样量10μl,流速1. 0 ml/min。结果 SBE_7-β-CD的保留时间为6. 8 min,主峰与相邻杂质峰分离度均不小于1. 94;方法的检测限为0. 32μg,定量限为0. 48μg; SBE_7-β-CD在0. 498 5～1. 495 mg/ml范围内线性关系良好(r=0. 999 8);方法精密度(n=6)的RSD为1. 4%;平均回收率(n=6)的平均值为98. 0%,RSD为1. 3%; 6批样品的含量为95. 8%～99. 3%。结论该方法准确度和重复性良好,适合SBE_7-β-CD的含量测定,为SBE_7-β-CD质量控制标准的建立奠定了基础。Objective To develop a method for the determination of SBE7-β-CD.Methods An HPLC method was employed.The sample was separated on a Phenomenex PolySep-GFC-P3000 column(7.8 mm×30 cm)at 35℃.A refractive index detector was used for the detection,and the detective temperature was 35℃.The mobile phase was a mixture of acetonitrile-0.1 mol/L potassium nitrate aqueous solution(35∶65)at a flow rate of 1.0 ml/min,and injection size was 10μl.Results The retention time of SBE7-β-CD was 6.8 min.The resolutions of sample and impurities were no less than 1.94;LOD and LOQ of this method were 0.32μg and 0.48μg;there was a good linear relationship of SBE7-β-CD at the range of 0.498 5~1.495 mg/ml(r=0.999 8);the precision of method(n=6)was 1.4%;the average of recovery was 98.0%and RSD was 1.3%;the content of 6 batches of samples was at the range of 95.8%~99.3%.Conclusion This method can be used for the determination of SBE7-β-CD for its accuracy and repeatability,which builds a solid foundation for the establishment of the quality standard of SBE7-β-CD.

关 键 词：SBE7-β-CD 辅料 平均取代度 高效液相色谱 含量测定 

分 类 号：R927.2[医药卫生—药学]