柱前衍生化HPLC法测定维U颠茄铝胶囊中维生素U的含量

发布时间：2018-01-06 08:39

本文关键词：柱前衍生化HPLC法测定维U颠茄铝胶囊中维生素U的含量　出处：《药物分析杂志》2016年07期 　论文类型：期刊论文

【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。
[Abstract]:Objective: to determination of vitamin U in vitamin U and aluminium capsules was improved, according to the special structure of vitamin U, the establishment of pre column derivatization and its content was determined by HPLC assay. Methods: two 4-dinitrofluorobenzene (FDNB) as a pre column derivatization reagent, sodium bicarbonate in carbonate buffer medium (pH 10) in the derivatization reaction; the content was determined by HPLC method using Agilent TC-C18 (250 mm * 4.6 mm, 5 m) column with 0.01 mol - L~ (-1) acetate solution (adjusted to pH 6.5 with acetic acid) - acetonitrile (70: 30) as mobile phase, flow rate of 1.0m - min~ (L -1), the detection wavelength of 360 nm. results: 2 kinds of structure of vitamin U (chloromethyl iodomethyl methionine and methionine) derivatives of chromatographic separation effects were good, chlorine methyl methionine and iodomethyl methionine concentration respectively in 20.12~201.20 and 29.23~292.31 g m L~ (-1) within the scope of a good linear relationship, chloromethyl methionine and iodine Recoveries of methyl methionine were 97.33%~98.74% and 97.71%~99.24%, RSD (n=6) were 1.95%~2.52% and 1.85%~2.78%; the content of vitamin U of different manufacturers measured the pre column derivatization HPLC of the 3 batches of samples were 99.06%, 99.73%, 100.52%, the content of the traditional titration measured were 101.07% 102.26%, 99.79%, two results are basically consistent. Conclusion: the method validation results show that this method can be used for the determination of vitamin U vitamin U belladonna aluminum capsule preparation.

【作者单位】：恩施土家族苗族自治州中心医院药剂科;仙桃市食品药品检验检测中心;
【分类号】：R927.2;O657.72
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