柱前衍生化HPLC法测定维U颠茄铝胶囊中维生素U的含量  

Determination of vitamin U in vitamin U,belladonna and aluminium capsules by pre-column derivatization HPLC

作　　者：马经明 赵吉平 

机构地区：[1]恩施土家族苗族自治州中心医院药剂科,恩施445000 [2]仙桃市食品药品检验检测中心,仙桃433000

出　　处：《药物分析杂志》2016年第7期1293-1298,共6页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:对维U颠茄铝胶囊中维生素U含量测定的方法进行改进,根据维生素U的特殊结构,建立柱前衍生化HPLC检测法测定其含量。方法:以二硝基氟苯(FDNB)为柱前衍生剂,在碳酸钠-碳酸氢钠缓冲液(pH 10.0)介质中进行衍生化反应;以HPLC法测定含量,采用Agilent TC-C18(250 mm×4.6 mm,5μm)色谱柱,以0.01 mol·L^(-1)乙酸钠溶液(用乙酸调pH至6.5)-乙腈(70∶30)为流动相,流速1.0m L·min^(-1),检测波长360 nm。结果:2种结构维生素U(氯甲基蛋氨酸和碘甲基蛋氨酸)的衍生产物色谱分离效果均良好,氯甲基蛋氨酸和碘甲基蛋氨酸质量浓度分别在为20.12~201.20和29.23~292.31μg·m L^(-1)范围内线性关系良好,氯甲基蛋氨酸和碘甲基蛋氨酸的加样回收率分别为97.33%~98.74%和97.71%~99.24%,RSD(n=6)分别为1.95%~2.52%和1.85%~2.78%;以本文的柱前衍生化HPLC法测得的不同厂家的3批样品中维生素U含量分别为99.06%、99.73%、100.52%,传统滴定法测得的含量分别为101.07%、102.26%、99.79%,两法结果基本一致。结论:方法学验证结果表明,本文建立的方法可以用于测定维U颠茄铝胶囊制剂中维生素U的含量。Objective：To establish a new analysis method for determination of vitamin U by pre-column derivatization HPLC according to vitamin U special structure,so as to improve the determination method of vitamin U in vitamin U,belladonna and aluminium capsules.Methods：The derivatization reaction is carried out in Na2CO3-Na HCO3 buffer（pH 10.0）medium,with dinitrofluorobenzene（FDNB）as pre-column derivatization,and then analyzed by HPLC.Agilent TC-C18（250 mm×4.6 mm,5 μm）column was adopted,the mobile phase consisted-of sodium acetate solution（adjusted to pH 6.5 with acetic acid）-acetonitrile（70∶30）at the flow rate of 1.0 mL ·min1,and the detection wavelength was 360 nm.Results：The derivation products of the two kinds of vitamin U （chlorine methyl methionine and idodine methyl methionine）could be well separated by HPLC.The results showed good rela-tionships between the ranges of 20.12-210.20 μg·m L-（-1）（chlorine methyl methionine）and 29.23-292.31 μg·m L1（idodine methyl methionine）.The recoveries for chlorine methyl methionine were 97.33%-98.74% and 97.71%-99.24% for idodine methyl methionine,and RSDs（n=6）were 1.95%-2.52% and 1.85%-2.78%.The vitamin U contents determined by pre-column derivatization HPLC of three samples from different companies were 99.06%,99.73% and 100.52%,while the contents by titration analysis method were 101.07%,102.26% and 99.79%.The results determined by two methods were almost the same.Conclusion：The established method is proved by methodology validation that it can be used for vitamin U determination in vitamin U,belladonna and aluminium capsules.

关 键 词：维U颠茄铝胶囊 维生素U 氯甲基蛋氨酸 碘甲基蛋氨酸 二硝基氟苯(FDNB) 衍生化 HPLC 

分 类 号：R917[医药卫生—药物分析学]