液液微萃取/固相微萃取-气相色谱法检测柑橘中16种游离氨基酸  

Determination of Sixteen Kinds of Free Amino Acids in Citrus by Liquid Liquid Microextraction/Solid Phase Microextraction Coupled with Gas Chromatography

作　　者：汪雨龙 李晓庆 李秀娟[3] WANG Yulong;LI Xiaoqing;LI Xiujuan(College of Pharmacopolist,Zhejiang Pharmaceutical University,Ningbo 315500,China;Jining Academy of Agricultural Sciences,Jining 272000,China;College of Food Science and Technology,Huazhong Agricultural University,Wuhan 430070,China)

机构地区：[1]浙江药科职业大学药商学院,浙江宁波315500 [2]济宁市农业科学研究院,山东济宁272000 [3]华中农业大学食品科学技术学院,湖北武汉430070

出　　处：《食品工业科技》2023年第12期285-292,共8页Science and Technology of Food Industry

基　　金：湖北省农业科技创新岗位项目(201962000000131);2021年浙江省市场监督管理局科技项目(ZC2021A044)。

摘　　要：目的:建立气相色谱氢火焰离子检测法同时测定柑橘果肉中16种游离氨基酸含量。方法:以对氯甲酸异丁酯为衍生剂,先进行衍生条件优化,再采用自制的溶胶-凝胶甲基丙烯酸丁酯二乙烯基苯涂层为萃取头,通过液液微萃取联合固相微萃取对样品进行前处理后上气相色谱仪检测。结果:对氯甲酸异丁酯衍生化柑橘中游离氨基酸采用一次性衍生法,衍生时间1 min。优化后的萃取温度为60℃,萃取时间30 min,离子强度为30%Na_(2)SO_(4),搅拌速度1000 r·min^(-1)。在此条件下,目标化合物具有良好的线性关系,相关系数均大于0.99,检出限为0.85~12.60μg·kg^(-1),相对标准偏差为2.51%~12.80%,三种加标浓度下回收率为82.51%~121.75%。结论:该方法操作简单、结果准确、受基质干扰少,适用于柑橘中多种游离氨基酸的检测,并可以游离氨基酸含量来评价柑橘内在品质。Objective:To evaluate the quality of the citrus,a gas chromatography(GC)coupled with flame ion detector was established for the determination of sixteen kinds of free amino acids in citrus simultaneously.Methods:Firstly,the single factor tests werre used to optimize the derivatization conditions of isobutyl chloroformate.Subsequently,a method was developed by liquid-liquid microextraction(LLME)/solid phase microextraction(SPME)coupled with GC using a home-made sol-gel butylmethacrylate/divinylbenzene(BMA/DVB)fibers.Results:The results showed that the derivatization conditions were the best under one derivation with one min.The best SPME conditions can be obtained as follows:The extraction temperature of 40℃,the extraction time of 30 min and the 30%sodium sulfate at the extraction speed of 1000 r·min^(−1).Under the optimized experimental parameters,there were good linear relationships for 16 analytes with correlation coefficients larger than 0.99.The limit of detection was 0.85~12.60μg·kg−1 and the standard recoveries of the spiked samples ranged from 82.51%to 121.75%,with relative standard deviations of 2.51%~12.80%.Conclusion:The method was convenient, accurate, and matrix resistant. It could be used as a new model for the determination of the free amino acids in citrus pulp samples and can also provide a valuable reference for the quality evaluation of cirtrus.

关 键 词：柑橘 游离氨基酸 液液微萃取(LLME) 固相微萃取(SPME) 气相色谱(GC) 

分 类 号：TS207.3[轻工技术与工程—食品科学]