正交试验优选维U颠茄铝胶囊中维生素U的HPLC柱前衍生条件  

Study on optimization of pre-column derivative reaction conditions of Vitamin U in Vitamin U Belladonna Aluminum Capsules by orthogonal design

作　　者：王林凤[1] WANG Linfeng(Affiliated Hospital of Shaanxi Traditional Chinese Medicine University, Shaanxi Province, Xianyang 712000, China)

机构地区：[1]陕西中医药大学附属医院,陕西咸阳712000

出　　处：《中国医药导报》2016年第34期42-45,49,共5页China Medical Herald

摘　　要：目的探索维U颠茄铝胶囊中维生素U的最佳衍生条件。方法选取二硝基氟苯（DNFB）为柱前衍生剂，以反应温度、介质pH、衍生剂DNFB与维生素U的摩尔比、反应时间4个考察因素设计L9（3^4）正交表安排试验，优选最佳工艺，并进行验证试验。在优选的条件下进行衍生反应，确定维生素U的含量测定方法。结果优选的衍生化反应条件为：反应温度70℃，介质pH=10．0，衍生剂DNFB与维生素U的摩尔比为1．3，反应时间40min。维生素U的两种构型分别在8～40μg／mL（r=0．9992）和12～60μg／mL（r=0．9997）浓度范围内线性关系良好。按照正交试验确定的最佳反应条件，对同一样品安排3次试验，衍生剂DNFB的转化率分刖为99．2％、99．5％、99．4％，表明该工艺稳定可行。结论该衍生方法简单方便、工艺稳定可行，可用于维生素U的柱前衍生-高效液相色谱测定。Objective To select the optimum pre-column derivative reaction conditions of Vitamin U in Vitamin U Belladonna Aluminum Capsules. Methods With dinitrofluorobenzene （DNFB） as the pre-cnlumn derivatization, and L9 （34） orthogonal test design was used to arrange sequent experiments to test the effects of four main factors including reaction temperature, pH, molar ratio of DNFB to Vitamin U and reaction time to establish optimal reaetion conditions. And the verification test was conducted. Then the method for determination of Vitamin U was established in the optimal reaction conditions. Results The optimal reaction conditions were as follows： reaction temperature 70℃, pH=10.0, the molar ratio of DNFB to Vitamin U was 1.3 and reaction time was 40 minutes. Two typs of Vitamin U had good linearity within the range of 8-40 ug/mL （r=0.9992） and 12-60 ug/mL（r=0.9997）. According to orthogonal experiment to deter- mine the optimum conditions for the same sample of 3 times, derivative agent DNFB conversion rates were 99.2%, 99.5% and 99.4% respectively, showed that the process was stable and viable. Conclusion The method is convenient and stable, and can be used for the determination of Vitamin U in Vitamin U Belladonna Aluminum Capsules by pre- column derivatization and HPLC.

关 键 词：维生素U 柱前衍生一高效液相色谱法:正交试验 

分 类 号：R917[医药卫生—药物分析学]