超高效合相色谱法测定火龙果果酒中游离氨基酸的含量
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摘要
建立超高效合相色谱测定食品中游离氨基酸的方法。选取Acquity UPC2Torus Diol(3.0 mm×100 mm,1.7μm)色谱柱,流动相由A(超临界二氧化碳)和B(V(甲醇)∶V(乙腈)=1∶1)组成,2.5 mmol/L乙酸铵作为改性剂,流速2.0 m L/min,紫外检测器波长280 nm,补偿范围330~430 nm,背压1 800 psi。结果表明,该方法具有良好的线性(R2=0.999 0~0.999 8),分离度高于1.22,检出限和定量限范围分别为23~57 ng/L和70~178ng/L,线性范围为20~400μg/m L,加标回收率在85.6%~101.2%之间。该方法被成功用于火龙果酒样品中游离氨基酸含量的测定,也为分析其他食品基质中游离氨基酸分布情况提供了新的方法。
A new method based on ultra performance convergence chromatography( UPC2) was developed for analysis of free amino acids in fruit wine. They were separated on an Acquity UPC2 Torus Diol( 3. 0 mm × 100 mm,1.7 μm) with a mobile phase consisted of supercritical CO_2 and methanol ∶ acetonitrile( 1∶ 1 v/v,with 2. 5 mmol/L ammonium acetate as mobile phase modifier). The flow rate was 2. 0 m L/min and DAD detection was set at 280 nm with a compensation range of 330-430 nm. Back pressure was 1 800 psi. The results showed good linearity( R2=0. 999 0-0. 999 8) and high resolution( > 1. 22). The limits of detection( LOD) and quantification( LOQ) ranged from 23-57 ng/L and 70-178 ng/L,respectively. The linear range was between 20 and 400 μg/m L. The spiked recoveries were ranged from 85. 6% to 101. 12%. It was applied for the free amino acids analysis of selected pitaya wine,which could also provide a new method for the analysis of free amino acid distribution in other food matrix from different sources.
A new method based on ultra performance convergence chromatography( UPC2) was developed for analysis of free amino acids in fruit wine. They were separated on an Acquity UPC2 Torus Diol( 3. 0 mm × 100 mm,1.7 μm) with a mobile phase consisted of supercritical CO_2 and methanol ∶ acetonitrile( 1∶ 1 v/v,with 2. 5 mmol/L ammonium acetate as mobile phase modifier). The flow rate was 2. 0 m L/min and DAD detection was set at 280 nm with a compensation range of 330-430 nm. Back pressure was 1 800 psi. The results showed good linearity( R2=0. 999 0-0. 999 8) and high resolution( > 1. 22). The limits of detection( LOD) and quantification( LOQ) ranged from 23-57 ng/L and 70-178 ng/L,respectively. The linear range was between 20 and 400 μg/m L. The spiked recoveries were ranged from 85. 6% to 101. 12%. It was applied for the free amino acids analysis of selected pitaya wine,which could also provide a new method for the analysis of free amino acid distribution in other food matrix from different sources.
引文
[1]吕雪娟,梁兰兰,黄华京,等.游离氨基酸含量对食品风味特征的影响[J].食品科学,1996,17(3):10-12.
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[3]薛敏,高贵田,赵金梅,等.不同品种猕猴桃果实游离氨基酸主成分分析与综合评价[J].食品工业科技,2014(5):294-299.
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[9]刘肖肖,李淑林,陆瑞利,等.液相色谱-电喷雾飞行时间质谱法同时测定虫生真菌菌丝中16种游离氨基酸[J].食品与发酵工业,2013,39(1):181-186.
[10]聂龙辉,王卫国.电喷雾质谱法对几种氨基酸的快速检测[J].分析试验室,2017,36(4):404-406.
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[13]分析测试百科.UPC2超高效合相色谱赋予科学家新的想象力[Z/OL].[2012-05-15].http://instrument.ofweek.com/2012-05/ART-8320088-8600-28612257.html.
[14]KRAUSE I,BOCKHARDT A,NECKERMANN H,et al.Simultaneous determination of amino-acids and biogenicamines by reversed phase high-performance liquid-chromatography of the dabsyl derivatives[J].Journal of Chromatography A,1995,715:67-79.
[15]REDRUELLO B,LADERO V,CUESTA I,et al.A fast,reliable,ultra high performance liquid chromatography method for the simultaneous determination of amino acids,biogenic amines and ammonium ions in cheese,using diethyl ethoxymethylenemalonate as a derivatising agent[J].Food Chemistry,2013,139:1 029-1 035.
[16]徐莉,禤开智,纪少凡,等.UPC2快速测定葡萄酒中抗坏血酸和异抗坏血酸含量研究[J].食品工业科技,2015,36(16):75-77.
[17]刘倩倩,周围,王波,等.超高效合相色谱法直接检测VC方法[J].食品科学,2014,35(16):208-211.
[18]ZHU Y C,LUO Y H,WANG P P.Simultaneous determination of free amino acids in Pu-er tea and their changes during fermentation[J].Food Chemistry,2016,194:643-649.
[19]车兰兰.液相色谱及液质联用法测定三种山西特色食品中游离氨基酸[D].太原:山西大学,2013:4-28.
[20]KORS A,VARGA Z,MOLNR-PERL I.Simultaneous analysis of amino acids and amines as their o-phthalaldehyde-ethanethiol-9-fluorenylmethyl chloroformate derivatives in cheese by high-performance liquid chromatography[J].Journal of Chromatography A,2008,1203(2):146-152.
[21]PEREIRA V,PONTES M,CMARA J S,et al.Simultaneous analysis of free amino acids and biogenic amines in honey and wine samples using in loop orthophthalaldeyde derivatization procedure[J].Journal of Chromatography A,2008,1 189(1):435-443.
[22]赵英莲,牟德华,李艳.2,4-二硝基氟苯柱前衍生HPLC检测树莓中游离氨基酸[J].食品科学,2015,36(6):178-182.
[23]BOSCH L,ALEGRIA A,FARRR.Application of the6-aminoquinolyl-N-hydroxysccinimidyl carbamate(AQC)reagent to the RP-HPLC determination of amino acids in infant foods.Journal of Chromatography B,2006,831(1):176-183.
[24]WANG Y Q,YE D Q,ZHU B Q,et al.Rapid HPLC analysis of amino acids and biogenic amines in wines during fermentation and evaluation of matrix effect[J].Food Chemistry,2014,163:6-15.
[25]吴小禾,龚霄.代谢组学在食品发酵研究中的应用现状及展望[J].中国食品学报,2011,11(9):220-224.
[2]黄艳.常见果蔬中游离氨基酸含量的测定[J].安徽农业科学,2013,41(9):4 088-4 089.
[3]薛敏,高贵田,赵金梅,等.不同品种猕猴桃果实游离氨基酸主成分分析与综合评价[J].食品工业科技,2014(5):294-299.
[4]刘婧琳,郭玉蓉.4种工艺苹果酒中的游离氨基酸及其呈味特征[J].陕西农业科学,2015,61(10):27-30,46.
[5]唐柯,马磊,徐岩,等.基于游离氨基酸水平对葡萄酒产地和品种的判别分析[J].食品与发酵工业,2015,41(9):159-163.
[6]GARDE-CERDN T,LORENZO C,LARA J F,et al.Study of the evolution of nitrogen compounds during grape ripening.application to differentiate grape varieties and cultivated systems[J].Journal of Agricultural&Food Chemistry,2009,57(6):2 410-2 410.
[7]YU H Y,ZHANG Y,XU C H,TIAN H X.Discrimination of wine age of Chinese rice wine by electronic tongue based on amino acid profiles[J].Transactions of the Chinese Society of Agricultural Engineering,2017,33(2):297-301.
[8]周远华,辛妮,胡育筑.氨基酸分析新技术在药学研究中的应用[J].药学进展,2011,35(11):503-508.
[9]刘肖肖,李淑林,陆瑞利,等.液相色谱-电喷雾飞行时间质谱法同时测定虫生真菌菌丝中16种游离氨基酸[J].食品与发酵工业,2013,39(1):181-186.
[10]聂龙辉,王卫国.电喷雾质谱法对几种氨基酸的快速检测[J].分析试验室,2017,36(4):404-406.
[11]徐永威,孙庆龙,黄静,等.沃特世超高效合相色谱系统—ACQUITY UPC2[J].现代科学仪器,2012,18(5):45-48.
[12]GONG X,QI N L,WANG X X,et al.Ultra-performance convergence chromatography(UPC2)method for the analysis of biogenic amines in fermented foods[J].Food Chemistry,2014,162:172-175.
[13]分析测试百科.UPC2超高效合相色谱赋予科学家新的想象力[Z/OL].[2012-05-15].http://instrument.ofweek.com/2012-05/ART-8320088-8600-28612257.html.
[14]KRAUSE I,BOCKHARDT A,NECKERMANN H,et al.Simultaneous determination of amino-acids and biogenicamines by reversed phase high-performance liquid-chromatography of the dabsyl derivatives[J].Journal of Chromatography A,1995,715:67-79.
[15]REDRUELLO B,LADERO V,CUESTA I,et al.A fast,reliable,ultra high performance liquid chromatography method for the simultaneous determination of amino acids,biogenic amines and ammonium ions in cheese,using diethyl ethoxymethylenemalonate as a derivatising agent[J].Food Chemistry,2013,139:1 029-1 035.
[16]徐莉,禤开智,纪少凡,等.UPC2快速测定葡萄酒中抗坏血酸和异抗坏血酸含量研究[J].食品工业科技,2015,36(16):75-77.
[17]刘倩倩,周围,王波,等.超高效合相色谱法直接检测VC方法[J].食品科学,2014,35(16):208-211.
[18]ZHU Y C,LUO Y H,WANG P P.Simultaneous determination of free amino acids in Pu-er tea and their changes during fermentation[J].Food Chemistry,2016,194:643-649.
[19]车兰兰.液相色谱及液质联用法测定三种山西特色食品中游离氨基酸[D].太原:山西大学,2013:4-28.
[20]KORS A,VARGA Z,MOLNR-PERL I.Simultaneous analysis of amino acids and amines as their o-phthalaldehyde-ethanethiol-9-fluorenylmethyl chloroformate derivatives in cheese by high-performance liquid chromatography[J].Journal of Chromatography A,2008,1203(2):146-152.
[21]PEREIRA V,PONTES M,CMARA J S,et al.Simultaneous analysis of free amino acids and biogenic amines in honey and wine samples using in loop orthophthalaldeyde derivatization procedure[J].Journal of Chromatography A,2008,1 189(1):435-443.
[22]赵英莲,牟德华,李艳.2,4-二硝基氟苯柱前衍生HPLC检测树莓中游离氨基酸[J].食品科学,2015,36(6):178-182.
[23]BOSCH L,ALEGRIA A,FARRR.Application of the6-aminoquinolyl-N-hydroxysccinimidyl carbamate(AQC)reagent to the RP-HPLC determination of amino acids in infant foods.Journal of Chromatography B,2006,831(1):176-183.
[24]WANG Y Q,YE D Q,ZHU B Q,et al.Rapid HPLC analysis of amino acids and biogenic amines in wines during fermentation and evaluation of matrix effect[J].Food Chemistry,2014,163:6-15.
[25]吴小禾,龚霄.代谢组学在食品发酵研究中的应用现状及展望[J].中国食品学报,2011,11(9):220-224.