分析测试学报2017,Vol.36Issue(6):778-782,5.DOI:10.3969/j.issn.1004-4957.2017.06.013
柱前衍生/高效液相色谱法测定果蔬中仲丁胺残留
Determination of 2-Aminobutane in Vegetables and Fruits by High Performance Liquid Chromatography Coupled with Pre-column Derivatization
摘要
Abstract
A high performance liquid chromatographic method with pre-column derivatization was developed for the determination of 2-aminobutane in vegetables and fruits.The sample was distilled with kjeldahl apparatus.The distillate was neutralized with NaOH solution before derivatization with 9-fluorenylemethyl chloroformate (FMOC) as derivatization agent under alkaline condition.The sample was separated on a C1s analytical column and detected by HPLC with a UV detector at a wavelength of 265 nm.Systematic investigation was carried out on the dependence of the dcrivatization conditions such as concentration of derivatization,pH value of borate buffer solution,reaction temperature and time etc.The optimized conditions were as follows:concentration of derivatization:0.50 g/L,pH value of borate buffer:8.0,reaction temperature:room temperature,and reaction time:10 min.Under the optimal conditions,a linear relationship was achieved between the peak area and the concentration of 2-aminobutane in the range of 0.001-1.000 mg/L,with a correlation coefficient of 0.999 8.The recoveries at three spiked levels were in the range of 82.4%-95.2% with relative standard deviations (RSDs) of 1.3%-6.8%.The limit of detection (LOD) was 0.1 μg/kg,and the limit of quantitation (LOQ) was 0.5 μg/kg.With the advantages of rapidness,simplicity,safety,high sensitivity and reproducibility,this method is suitble for the determination of 2-aminobutane in vegetables and fruits.关键词
柱前衍生/高效液相色谱/全自动凯氏定氮仪/仲丁胺/果蔬Key words
pre-column derivatization/high performance liquid chromatography (HPLC)/kjeldahl apparatus/2-aminobutane/vegetables and fruits分类
化学化工引用本文复制引用
周蓉,曹赵云,赵肖华,林晓燕,牟仁祥..柱前衍生/高效液相色谱法测定果蔬中仲丁胺残留[J].分析测试学报,2017,36(6):778-782,5.基金项目
浙江省科技计划项目(2015C37057) (2015C37057)