柱内光纤发光二极管诱导荧光检测毛细管电泳测定药片中的硫胺素

Determination of Thiamine of Capillary Electrophoresis with In-column Fiber-optic Light-emitting Diode-induced Fluorescence Detection

建立了毛细管电泳柱内光纤发光二极管诱导荧光检测法(CE-ICFO-LED-IFD)测定维生素B1药片中硫胺素含量的方法。以380 nm紫外发光二极管作为激发光源,采用光纤传导激发光至检测窗口。硫胺素在电泳分析前,经铁氰化钾溶液衍生。对各种影响电泳检测硫胺素的因素进行考察,最佳电泳条件为:硼砂缓冲液浓度为10 mmol/L、缓冲液为pH8. 4、分离电压为22 kV。硫胺素在0.05~25μmol/L范围内具有良好的线性关系(r=0. 999 4),最低检出限为11nmol/L。迁移时间和峰高的相对标准偏差(RSD)分别为1. 18%和3. 09%。加标回收率为98. 3%~106. 7%,RSD为2. 55%~3. 59%。维生素B1药片中硫胺素含量为9.88 mg/62. 0 mg。该方法简便、快速、准确可靠、成本低、灵敏度高,为完善维生素B1药片质量控制提供了新的方法和依据。

A home-build capillary electrophoresis with in-column fiber-optic light-emitting diode-induced fluorescence detection( CE-ICFO-LED-IFD) was developed for the determination of thiamine.A 380 nm ultraviolet light-emitting diode( UV-LED) was used as excitation light source and an optical fiber was used to guide the excitation light into the capillary right at the detection window.Thiamine was precolumn-derivatized with potassium ferricyanide.The influence of buffer concentration,buffer p H and applied voltage was systematically investigated.Optimal separation conditions were obtained with 10 mmol/L borate buffer at p H 8. 4 and an applied voltage of 22 kV.The thiamine had a good linear relationship in the concentration ranges of 0. 05 ~ 25 μmol/L( r =0. 999 4) and the limit of detection( LOD) was 11 nmol/L. The relative standard deviations of migration time and peak height were 1. 18% and 3. 09%,respectively. The average recoveries were 98. 3%~ 106. 7% with the RSDs ranging from 2. 55% to 3. 59%.The content of thiamine in the Vitamin B1 tablets was 9. 88 mg/62. 0 mg. The proposed method is simple,fast,accurate and low-cost which provides a new method and basis for improving the quality control of Vitamin B1 tablets.