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李晓庆,蔡颖,潘思轶,李秀娟.氯甲酸异丁酯二次衍生气相色谱法检测柑橘中游离氨基酸[J].华中农业大学学报,2020,39(2):122-132
氯甲酸异丁酯二次衍生气相色谱法检测柑橘中游离氨基酸
Analysis of free amino acids in citrus by gas chromatography after isobutyl chloroformate second derivatization
投稿时间:2019-09-25  
DOI:
中文关键词:  柑橘; 游离氨基酸; 氯甲酸异丁酯; 二次衍生; 超声提取; 气相色谱  定量检测
英文关键词:citrus  free amino acid  isobutyl chloroformate  second derivatization  ultrasonic extraction  gas chromatography  quantitative detection
基金项目:湖北省农业科技创新岗位项目 (201962000000131)
作者单位E-mail
李晓庆 华中农业大学食品科学技术学院武汉 430070 1535678395@qq.com 
蔡颖 华中农业大学食品科学技术学院武汉 430070  
潘思轶 华中农业大学食品科学技术学院武汉 430070  
李秀娟 华中农业大学食品科学技术学院武汉 430070 lixiujuan@mail.hzau.edu.cn 
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中文摘要:
      采用单因素试验法对氯甲酸异丁酯二次衍生条件进行优化,并建立了1种柑橘果肉中18种游离氨基酸的气相色谱定量检测方法。结果显示:当吡啶、异丁醇、第1次氯甲酸异丁酯和第2次氯甲酸异丁酯加入量分别为20、120、50和50 μL,萃取溶剂为二氯甲烷时,氨基酸衍生效果最佳;18种氨基酸在其对应范围内线性关系良好,相关系数R2均大于 0.99,检测限在0.02~0.35 μg/mL,5次重复试验相对标准偏差不超过 10.57%;5种柑橘提取液样品的加标回收率均在 72.82%~132.97%。该方法简便、准确、重现性好、成本低,衍生物稳定,可以用于柑橘果肉中18种游离氨基酸的检测。
英文摘要:
      In this paper,the single factor test was used to optimize the second derivatization conditions of isobutyl chloroformate,and a gas chromatography quantitative detection method for 18 free amino acids in citrus pulp was established. The results showed that the analysis conditions were the best when pyridine,2 methyl 1 propanol,first isobutyl chloroformate and second isobutyl chloroformate were added in the amount of 20 μL,120 μL,50 μL and 50 μL,respectively,and the extraction solvent was dichloromethane. The 18 amino acids showed good linearities in their respective linear ranges,and the correlation coefficient R2 were greater than 0.99. The detection limits were in the range of 0.02-0.35 μg/mL,and the relative standard deviations of 5 repeated tests were no more than 10.57%. The recoveries in five kinds of citrus extracts were between 72.82% and 132.97%. The method is simple,accurate,reproducible,low in cost,stable in derivatives,which can be used for the detection of 18 free amino acids in citrus pulp.
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