柱前衍生化HPLC检测硫酸卡那霉素的方法研究

目的 采用柱前衍生化高效液相色谱法建立了快速定性、定量分析食品中的硫酸卡那霉素的方法。方法 首先茚三酮-吡啶溶液作为衍生化试剂考察了衍生化反应条件。包括反应溶液的酸碱度、温度和反应时间，并建立了色谱分离条件。衍生化条件为在pH为5．8条件下,75℃水浴中反应20min。色谱条件为，色谱柱：150×4．6mm Kramasd C18；流动相：甲醇-水（40：60）；流速：O．5mL·min^-1；紫外检测波长390nm；进样量：20μL。结果 硫酸卡那霉素的浓度在2．24×10^-5mol·L^-1～1．12×10^-4mol·L^-1之内，浓度与峰面积呈现良好的线性关系，建立的方法线性良好,样品回收率在95％～98~%之间。结论 本方法快速、灵敏,适合日常样品检测的需要。

Studies of Kanamycin sulfate determination method by HPLC with precolumn derivatization

OBJECTIVE The use of pre-column derivatization HPLC method to establish a rapid qualitative and quantitative analysis of kanamycin sulfate method in food. METHODS First of all, Ninhydrin-pyridine solution as derivatization reagent inspected derivatization reaction conditions, including the reaction solution pH, temperature and reaction time, and the establishment of the conditions of chromatographic separation. Derivatization conditions in pH 5.8, under 7512 reaction for 20 minutes. Chromatographic conditions were as follows： 150 × 4.6 mm Kromasil C18; mobile phase： methanol-water（40 ： 60） ; flow rate： 0.5mL·min^-1; UV detection at 390nm; injection volume：20μL. RESULTS The Kanamycin sulfate concentration and peak area showed a good linear relationship in the range of 2.24 × 10^-5mol·L^-1 - 1.12 ×10^-4mol· L^-1, and the recoveries was at 95% - 98%. CONCLUSION The method is rapid, sensitive and suitable for realy sample testing.