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1 6 12 Vol. 6 No Journal of Food Safety and Quality Dec., 2015 卢斌斌 1, 李娟 2, 李鹏 1, 曾世通 1, 张璟琳 2, 孙世豪 1, 黄明泉 (1., ; 2.,, ; 3.,, ) 2, 3* 摘要 : 目的, 方法 11 16, (Asp) (Glu) (Phe) 结果 11, 4.52~ mg/100 g ;, mg/100 g,, mg/100 g,, mg/100 g;, 4.52 mg/100 g;, ;,,,,, 结论 11, 关键词 : ; ; ; ; ; Determination of amino acids composition in tobacco flavor concretes LU Bin-Bin 1, LI Juan 2, LI Peng 1, ZENG Shi-Tong 1, ZHANG Jing-Lin 2, SUN Shi-Hao 1 2, 3*, HUANG Ming-Quan (1. Zhengzhou Tobacco Research Institute, China Tobacco Company, Zhengzhou , China; 2. School of Food and Chemical Engineering, Beijing Technology and Business University, Beijing , China; 3. Beijing Laboratory for Food Quality and Safety, Beijing Technology and Business University, Beijing , China) ABSTRACT: Objective To detect amino acids composition in tobacco flavor concretes in order to provide reference data for safe use and tobacco extract standards. Methods Sixteen amino acids (such as aspartic acid, glutamic acid, and L-phenylalanine) were determined in natural tobacco concretes by hydrochloric acid hydrolyzation and automatic amino acid analyzer. Experimental data were analyzed by ANOVA and cluster analysis. Results The amount of amino acids in the tobacco flavor concretes was low, among 4.52~ mg/100 g; the average total amount of amino acids in Siraitia grosvenorii concrete was mg/100 g and significantly higher than other concretes, the highest of total amino acid amount was mg/100 g from Mangosteen extract of Aipu, and the aspartic acid content and glutamic acid content were higher than other 基金项目 : ( ) (CIT & TCD ) Fund: Supported by the National Natural Science Foundation of China ( ), and Importation and Development of High-Caliber Talents Project of Beijing Municipal Institutions(CIT & TCD ) * 通讯作者 :,,, hmqsir@163.com *Corresponding author: HUANG Ming-Quan, Associate Professor, Beijing Technology and Business Universtiy, No.11, Fucheng Road, Haidian District, Beijing , China. hmqsir@163.com

2 12, : 4909 amino acid, mg/100 g and mg/100 g, respectively. The total amount of amino acid in West Lake Ruta graveolens concrete was the minimum, 4.52 mg/100 g. Through factor analysis of variance, it was found that there were significant differences in the amounts of the same amino acid from different concretes. These concretes were divided into 2 categories by cluster analysis according to the total amount from amino acid, and Mangosteen extract from West Lake and Yancao, Hops extract from West Lake, Hawthorn extract, Wolfberry extract from Jishui and Rue extract were classified as one category, Mangosteen Extract from Tuopu and Aipu, and West Lake Wolfberry extract were the other. Conclusion The amount of amino acids in the 11 kinds of tobacco flavor concretes is low, and there are significant differences in the amounts of the same amino acid from different concretes. KEY WORDS: amino acid; tobacco flavor concretes; amino acid analyzer; hydrochloric acid hydrolyzed; factor analysis of variance; cluster analysis 1 引言, [1],,, [2], [3],,, [4-9], [10-11],,,, [12-14],,, 1958 Spackman [15],,, [16-18], ( ) ( ) -,,, 2 材料与方法 2.1 材料与试剂 11,, 1~11, 1 ( (Cys) 1.25 mmol/l, 2.5 mmol/l)(sigma ); (, ) 2.2 仪器与设备 30+ ( Biochrom ); Pipetman M ( : 100~1000 μl, Gilson ); T-403 ( g, ); RE-52AA ( ); WG9220A ( ) 2.3 实验方法样品前处理 g, 7 ml 6 mol/l, 5 min, 110, 24 h,,, 10 ml 2.00 ml 50 ml,, 1.00 ml

3 Table 1 表 1 11 种浸膏样品信息表 Information of 11 kinds of concrete samples ,, 1.00 ml Sodiun Loading Buffer, 0.45 μm, [19] 定性定量方法 : : Sodiun Loading Buffer mmol/l,, 3, 检测条件 Biochrom Na, 4.6 μm 200 mm; nm; 35.0 ml/h; 45~98 ; 135 ; 25.0 ml/h; 20 μl 统计分析 SPSS17.0(IBM, ), Duncan,,, 3 结果与讨论 3.1 标准曲线及相关系数 17 ( Cys) 1, nm, Pro, 440 nm, Pro,,, 16 ( Cys),, 2 2, 0.99, 3.2 精密度实验, 6, (RSD), 3 3, 16 RSD 0.64%~2.29% (n=6),,

4 12, : 4911 Fig. 1 1 Chromatogram of liquid standard mixture of amino acid 表 2 16 种氨基酸的回归方程与相关系数 Table 2 The regression equations and correlation coefficient values of 16 amino acids Table 3 表 3 氨基酸混标精密度分析结果 RSD values of mixed standard amino acids Asp Y=4.4422X Thr Y=3.6491X Ser Y=5.6731X Glu Y=4.1656X Pro Y=1.9369X Gly Y=5.1457X Ala Y=4.6026X Val Y=4.3356X Met Y=4.867X Ile Y=4.1966X Leu Y=4.9995X Tyr Y=5.3236X Phe Y=5.5514X His Y=6.506X Lys Y=6.4848X Arg Y=6.0778X (mv) RSD(%) Asp ± Thr ± Ser ± Glu ± Pro ± Gly ± Ala ± Val ± Met ± Ile ± Leu ± Tyr ± Phe ± His ± Lys ± Arg ± 重复性实验 6,, 2, 4 2, 4,,, 16 RSD 5%,, 种浸膏中氨基酸定量分析结果 11, 5 5,, 11,, 5 16, 6,

5 (Met), 5 ; (Thr) (Pro) (Tyr), 10, mg/100 g;, mg/100 g mg/100 g,, 4.52 mg/100 g (Pro) (Tyr), 10, mg/100 g, mg/100 g,, RSD 10%,, 11, 3, 2, 3~8 10~11,,,,,, 1~2 9 (6~8), Fig. 2 2 Chromatogram of each amino acid in West Lake Hops extract 表 4 西湖啤酒花浸膏中各氨基酸定量分析重复性实验 Table 4 Results of repeatability experiment of West Lake Hops extract ± (mg/100 g ) (RSD, %) Asp ± Thr 13.17± Ser 18.91± Glu 97.17± Pro 16.28± Gly 33.84± Ala 57.98± Val 43.71± Met - - Ile 27.82± Leu 30.35± Tyr 29.41± Phe 20.17± His 3.57± Lys 7.59± Arg 15.89± : μmol/ml, Fig Dendrogram obtained by cluster analysis of 11 kinds of concretes based on Table 5

6 12, : 4913

7 4914 6, (5) (10),,,,,, 4 结论 (Asp Thr Ser Glu Gly Ala Val Met Ile Leu Tyr Phe His Lys Arg), (, 60~80 mg/g DW [21] ); ;, ;, ;,, [20], ;,, (, ),, 参考文献 [1],,. [M]. :, Xie JP, Hu QY, Liu T. Domestic and foreign tobacco additives laws and regulations [M]. Beijing: Chemical Industry Press, [2],. [M]. :, Sun BG, He J. Perfume chemistry and technology [M]. Beijing: Chemical Industry Press, [3],,,. [J]., 2004, 20(2): Zhong HX, Cai JB, Yang DH, et al. Comparison of extraction methods for analysis of aroma components in tobacco concrete [J]. J Anal Sci, 2004, 20(2): [4],,,. SDE/GC-MS [J]., 2005, 24(6): Wu D, Song GX, Chen ZF, et al. Analysis & researeh of volatile compounds in tobacco concrete with SDE/GC-MS method [J]. J Instrum Anal, 2005, 24(6): [5] 堃. - - [J]., 2004, 25(4): Liao K. Analysis of volatile components in concrete by solid phase microextraction gas chromatography-mass spectrometry [J]. J Chin Mass Spectrom Soc, 2004, 25(4): [6],,,. GC/MS [J]., 2014, (7): Zhang YF, Bao FW, Chen WH, et al. Fingerprint spectra of GC/MS of tobacco flavor [J]. Tobacco Chem, 2014, (7): [7],,,. [J]., 2011, 28(5): Ji XM, Zhao XH, Li BJ, et al. Analysis of volatile components in Trollius chinensis bunge extract and its application in cigarette flavoring [J]. Fine Chem, 2001, 28(5): [8] Om Prakas, Rout PK, Chanotiya CS, et al. Composition of essential oil, concrete, absolute and SPME analysis of Tagetes patula capitula [J]. Ind Crops Prod, 2012, 37: [9],,,. GC/MS [J]., 2013, (7): Xie QT, Li JJ, Wang KB, et al. Analysis of volatile components in tieguangyin tea stem concrete by GC/MS and its application in cigarette [J]. Tobacco Chem, 2013, (7): [10],,,. 6 [J]., 2011, 29(10): Cai XM, Xia L, Sun YS, et al. Analysis of six acidic components in hops extracts by high performance liquid chromatography [J]. Chin J Chromatogr, 2011, 29(10): [11],,,. HPLC 3 [J]., 2010, 30(6): Jiang WH, Liu J, Zhong ZQ, et al. Simultaneous determination of 3 components in Ciwujia extractum by HPLC [J]. Chin J Pharm Anal, 2010, 30(6): [12],,,. [J]., 2004, (8):

12, : 4915 Zhang JS, Jia CX, Li YQ, et al. Determination of free amino acids in tobacco with automatic analyzer [J]. Tobacco Chem, 2004, (8): 26 32. [13] Li G, Wu D, Xie WY, et al.

8 12, : 4915 Zhang JS, Jia CX, Li YQ, et al. Determination of free amino acids in tobacco with automatic analyzer [J]. Tobacco Chem, 2004, (8): [13] Li G, Wu D, Xie WY, et al. Analysis of amino acids in tobacco by derivatization and dispersive liquid liquid microextraction based on solidification of floating organic droplet method [J]. J Chromatogr A, 2013, 1296: [14],,,. - [J]., 2014, (3): Deng QX, Xie W, Huang CZ, et al. Determination of amino acids in tobacco flavors by liquid chromatography tandem mass spectrometry [J]. Tobacco Chem, 2014, (3): [15] Spackman DH, Stein WH, Moore S. Automatic recording apparatus for use in the chromatography of amino acids [J]. Anal Chem, 1958, 30(7): [16] Yoshida Kazuo, Hasegawa Tetsuya, Haraguchi Hiroki. Determination of amino acids by liquid chromatography with inductively coupled plasma atomic emission spectrometric detection [J]. Anal Chem, 1983, 55: [17] Nolan TG, Hart BK, Doviehi NJ. Photothermal refraction as a microbore liquid chromatography detector in femtomde amino acid determination [J]. Anal Chem, 1985, 57: [18] Dobashi A, Hara S. Optical resolution of the D- and L-amino acid derivatives by silica gel liquid chromatography with chiral additive N-acetyl-L-valine tert-butylamide [J]. Anal Chem, 1983, 55: [19] GB/T [S]. GB/T Determination of amino acids in foods [S]. [20],. [J]., 2011, 39(8): Zhang H, Li XH. Research progress on chemical compositions of Fructus Momordicae [J]. J Anhui Agric Sci, 2011, 39(8): [21],,. [J]., 1988, (3): Wang SS, Wang BH, Li XZ. Progress in relation to leaf quality and variation of amino acids in tobacco [J]. Chin Tobacco Sci, 1988, (3): 作者简介 ( 责任编辑 : 杨翠娜 ) 卢斌斌, 高级工程师, 主要研究方向为香精香料检测分析与安全评价 lubb@ztri.com.cn 黄明泉, 博士, 副教授, 主要研究方向为香料香精食品检测与分析 hmqsir@163.com

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i i ii 1 2 3 4 % N) 5 50.0 AMINO ACID #64 [modified by Administrator] IntAmp_1 nc 40.0 30.0 20.0 10.0 0.0-10.0 1 - ala - 10.483 2 - thr - 11.107 3 - gly - 11.872 4 - val - 13.458 5 - ser - 14.903 6 - pro