摘要
建立了一种高效液相色谱-蒸发光散射检测法(HPLC-ELSD)同时测定阿胶和阿胶汁中4种主要未衍生化氨基酸(L-甘氨酸、L-羟脯氨酸、L-丙氨酸、L-脯氨酸)含量的方法,从源头对阿胶进行质量控制。采用6 mol·L^(-1)的盐酸对经真空干燥后的阿胶及阿胶汁粉末110℃恒温水解24 h,以Thermo hypercarb(150 mm×4.6 mm,5μm)为分析柱,流动相A为0.08%三氟乙酸甲醇∶乙腈(90∶10),B为2 mmol·L^(-1)全氟戊酸水,梯度洗脱,流速为0.8 m L·min^(-1)。结果表明,L-甘氨酸、L-羟脯氨酸、L-丙氨酸、L-脯氨酸的质量浓度与峰面积呈良好的线性关系(r>0.9993),阿胶与阿胶汁的加标回收率分别为97.42%~103.29%、97.17%~102.19%,RSD均<2.46%(n=6)。此方法简单快速、重复性较好,适用于快速准确地测定阿胶和阿胶汁中L-甘氨酸、L-羟脯氨酸、L-丙氨酸、L-脯氨酸含量,为其质量控制提供参考。
An analytical method for the determination of non-derivatized amino acids by HPLC- ELSD was developed. The contents of L- glycine （ Gly）, L- hydroxyproline （ Hyp ）, L- alanine （Ala） and L- proline （ Pro ） in CoUa Corii Asini and donkeyhide gelatin juice were determined simultaneously. The dried Colla Corii Asini and donkey-hide gelatin juice powder were hydrolyzed with 6 mol·L-1 hydrochloric acid at 110 ℃ for 24 h and then analyzed by Thermo hyperearb （ 150 mm x 4.6 mm, 5μm） with methanol-acetonitrile solution containing 0.08% trifluoroacetic acid （90：10）as mobile phase A and water containing 2 mmol·L-1 perfluorovalerate as mobile phase B with a flow rate of 0.8 mL·min-1 under the gradient elution.The carrier gas flow rate was 1.5 L· min-1 and the temperature of drift tube was 55 ℃ .As the results, the four amino acids were completely separated and there was a good linearity in the certain range （r 〉 0.9993 ）.The average recoveries of four amino acids were 97.42%-103.29% and 97.17%-102.19% in the donkey-hide gelatin and donkey-hide gelatin juice respectively with RSD 〈2.46% （n = 6 ）.The developed method was simple, precise and good reproducibility. It could be used to quickly and accurately determine the content of four underivatized amino acids in donkey-hide gelatin and donkey-hide gelatin juice, which was suitable for the quality control of CoUa Corii Asini.
作者
姜姣姣
王涛
张敏敏
刘倩
时新刚
王晓
JIANG Jiao-jiao;WANG Tao;ZHANG Min- min;LIU Qian;SHI Xin- gang;WANG Xiao(Qilu University of Technology（ Shandong Academy of Sciences） , Shandong Analysis and Test Center, Shandong Key Laboratory of TCM Quality Control Technology, Jinan 250014, China;Shandong University of Traditional Chinese Medicine, Jinan 250355, China)
出处
《食品工业科技》
CAS
CSCD
北大核心
2018年第13期257-261,共5页
Science and Technology of Food Industry
基金
山东省分析测试中心科技发展基金项目(山分基合字2015第6号)
国家自然基金(21506119,81603286)
山东省三院联合基金(ZR2016YL006).
关键词
阿胶
阿胶汁
氨基酸
非衍生化
HPLC-ELSD
Colla Corii Asini
donkey- hide gelatin juice
amino acid
non- derivatized
HPLC- ELSD
