Microsoft Word 张莉莉_二校出4023

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1 7 10 Vol. 7 No Journal of Food Safety and Quality Oct., 张莉莉, 孙颖, 孔琰, 杨肖, 张玉玉 *, 孙宝国, 陈海涛 (,,,, ) 摘要 : 目的 5- 方法, : Venusil XBP-C 18, UV 284 nm, - (5:95, V:V), 1.0 ml/min, 30 结果 25 min 5-HMF 0.16~40.00 µg/ml, r 2 =0.9999, μg/l, 2.82 μg/l 5-HMF %, 5-HMF 7.80 mg/kg, 5-HMF mg/kg, RSD 5% 结论, 5- 关键词 : ; 5- ; Content determination of 5-hydroxymethylfurfural in meat flavors ZHANG Li-Li, SUN Ying, KONG Yan, YANG Xiao, ZHANG Yu-Yu *, SUN Bao-Guo, CHEN Hai-Tao (Beijing Advanced Innovation Center for Food Nutrition and Human Health, Beijing Laboratory for Food Quality and Safety, Beijing Key Laboratory of Flavor Chemistry, Beijing Technology and Business University, Beijing , China) ABSTRACT: Objective To establish a method for the determination of 5-hydroxymethylfurfural in meat flavors by high performance liquid chromatography (HPLC). Methods The flavor samples were extracted with methanol and then centrifuged, and after being filtered, the supernatant fluid obtained was analyzed by HPLC. The samples were analyzed on a Venusil XBP-C 18 column at 284 nm with a UV detector. Using the methanol water solution (5:95, V:V) as mobile phase with the flow rate was 1.0 ml/min and the column temperature was 30. Results The separation and analysis of the target compound were accomplished within 25 min using this method. The 5-HMF standard had a good linear relationship in the range of 0.16~40.00 µg/ml with r 2 =0.9999, the limits of detection (LOD) was μg/l, and the limit of quantitation (LOQ) was 2.82 μg/l. The average recoveries at 3 additional levels was 86.89%, which could meet the requirements of sample determination. The content of 5-HMF in homemade sweet and sour spareribs flavor was 7.80 mg/kg, the average content of 5-HMF in pork flavor, beef flavor and chicken flavor sold in markets were 3.94, 5.32 and 9.38 mg/kg, and the average relative standard deviations of the results were all less than 基金项目 : (2016YFD ) ( ) (2014BAD04B06) Fund: Supported by the National Key R&D Program (2016YFD ), the National Natural Science Foundation of China ( ), and the National Key Technology R&D Program (2014BAD04B06) * 通讯作者 :,, zhangyy2@163.com *Corresponding author: ZHANG Yu-Yu, Associate Professor, School of Food and Chemical Engineering, Beijing Laboratory for Food Quality and Safety, Beijing Technology and Business University, Beijing , China. zhangyy2@163.com

2 %. Conclusion The proposed method is fast, accurate and sensitive, which is suitable for the quantitative analysis of 5-HMF in meat flavors. KEY WORDS: meat flavor; 5-hydroxymethylfurfural; high performance liquid chromatography 1 引言 5- (5-hydroxymethylfurfural, 5-HMF) [1],, [2,3] [4,5] [6] [7] [8,9] [10] [11,12], 5-HMF, 5-HMF, [13,14] 5-HMF, [15] GB/T [16], 5-HMF 40 mg/kg GB/T [17], 5-HMF 20 mg/kg, 5-HMF (high performance liquid chromatography, HPLC) [18], [19] HMF, 5-HMF ; [20], 5-HMF, 5-HMF ; [21] 5-HMF, 5-HMF, [20], 5-HMF ; [22] 40 ph 5-HMF, ph 5-HMF ; [23] 3 5-HMF, 5-HMF 5-HMF, 2 材料与方法 2.1 试剂与仪器 5,, ; (, ); 5- ( 99%,, Sigma ); (, Fisher ); ( ); 0.45 μm ( ) 1260 ( Quat Pump ALS TCC DAD OpenLAB CDS, ); Venusil XBP-C 18 (L) (4.6 mm 250 mm, 5 µm, ); 3K15 ( Sigma ) 2.2 实验方法 [24] 糖醋排骨香精的制备 2 cm,, m( ):m( )=1:2,, 50, 0.2%( ) 3 h,, 90, 10 min,, 74~150 µm, m( ):m( )=2:1, m( ):m( )=1:1,, 50, 0.2% ( ) 3 h,, 90, 10 min,, 0.11 MPa, min, : 4.40 ml 7.60 g 5.00 g 1.00 g 0.90 g 7.20 g 1.35 g (HVP ) 0.16 g (I+G) 0.27 g (VB 1 ) 0.73 g 0.73 g 0.73 g 0.73 g : m( ):m( ):m( ):m( ):m( ):m( ):m( ):m( ):m( )=4:1:4:8:8:1:2:2:8( 0.10%) g g : 0.11~0.12 MPa, 121~123, 15 min 标准溶液的配制 5-HMF g,, 100 ml, 286 µg/ml 5-HMF, 样品溶液的配制 4, 20 g, 4, 9600 r/min 10 min, 3, 1:1(V:V),

3 10, : min, 9600 r/min, 4 30 min,, 0.45 µm, 测定条件 : Venusil XBP-C 18 (4.6 mm 250 mm, 5 μm); 30 ; UV, 284 nm; 5%( ), ; 1.0 ml/min; 20 μl 3 结果与分析 3.1 色谱流动相的优化 5% 10% 15%(V:V) -,, 284 nm, 1.0 ml/min, 5% -, 5-HMF 5-HMF 1 2 2, 5-HMF 3.2 标准曲线和线性范围 286 µg/ml 5-HMF µg/ml 0.45 µm, HPLC, 3, 5-HMF, 5-HMF, 3, Y=719.03X , r 2 =0.9999, 5-HMF 0.16~40.00 µg/ml, 5-HMF Fig HMF The high performance liquid chromatogram of 5-HMF standard solution Fig. 2 2 The high performance liquid chromatogram of extract from homemade sweet and sour spareribs flavor

4 , 3 RSD 5%, 表 1 方法的重复性考察 (n=3) Table 1 Repeatability of the method (n=3) 5-HMF (mg/kg) RSD(%) RSD(%) HMF Fig. 3 Standard curve of 5-HMF 3.3 方法的检出限和定量限 S/N=3 (detection limit, LOD), S/N=10 (limit of quantitation, LOQ) 9, 5-HMF LOD= μg/l, LOQ=2.82 μg/l 3.4 方法的重复性 3, 1.0 ml, 3, HMF, (relative standard deviation, RSD),, 3.5 精密度实验, 2.86 mg/l mg/l mg/l 5-HMF, 6, 2 2, 3 5-HMF RSD 5%, 3.6 加标回收率实验 5-HMF 9, ml 5-HMF (286 µg/ml), 5-HMF, 5-HMF, 3 3, 5-HMF 80%~120%, RSD 5%, 表 2 Table 2 方法的精密度考察 (n=6) Precision of the method (n=6) 5-HMF (mg/l) 5-HMF RSD(%) RSD(%) 表 3 5-HMF 的回收率 (n=3) Table 3 The recoveries of 5-HMF (n=3) /ml 5-HMF /µg 5-HMF /µg 5-HMF /µg /% RSD (%)

5 10, : 表 4 样品中 5-HMF 的含量 (n=3) Table 4 The contents of 5-HMF in samples (n=3) HMF (mg/kg) RSD (%) 3.41±0.07 a 3.31±0.15 b n.d. 6.29±0.01 c 2.74±0.04 d ±0.06 f 3.09±0.03 h 2.45±0.05 i 13.91±0.02 j 5.12±0.08 k ±0.12 a 8.92±0.16 c 14.31±0.13 d 2.96±0.03 j 15.33±0.57 n ± : n.d. ; 5-HMF ( ± ) ; (P<0.05) 3.7 样品测定 2.2.3, 5-HMF, 4 4, 5-HMF 0~15.33 mg/kg, ph 5-HMF 15 11, [25],,, 5-HMF 4 结论 5-HMF, : - (5:95, V:V), 1.0 ml/min, Venusil XBP-C 18, 30, UV 284 nm 5-HMF 0.16~40.00 µg/ml,, r 2 =0.9999, μg/l, 2.82 μg/l,, 5-HMF 7.80 mg/kg, 5-HMF mg/kg, RSD 5% 5-HMF, 参考文献 [1],. 5- [J]., 2013, 38(1): Zhang YL, Zhou WQ. Investigation of the correlation between content and antioxidant activities of Maillard reaction product-5-hmf [J]. China Condim, 2013, 38(1): [2] Chen L, Huang H, Liu W, et al. Kinetics of the 5-hydroxymenthylfurfural formation reaction in Chinese rice wine [J]. J Agric Food Chem, 2010, 58(6): [3],,,. [J]., 2015, 37(5): Zhong L, Wang YW, Yang SL, et al. Connection of stewing Rehmanniae Radix with wine and its taste [J]. Chin Tradit Patent Med, 2015, 37(5): [4] Ajlouni S, Sujirapinyokul P. Hydroxymenthylfurfuraldehyde and amylase contents in Australian honey [J]. Food Chem, 2010, 119(3): [5],,,. HPLC 6 5- [J]., 2012, 25(6): Long GM, Qiu L, Ma L, et al. Determination of 5-HMF content in 6 different kinds of honey by HPLC [J]. J Math Med, 2012, 25(6): [6] Akpɪnar K, Karakaş B, Akça H, et al. Determination of HMF in roasted flour/oil mixtures and effect of solvent used in the extraction procedure [J]. Food Chem, 2011, 128(3): [7],,,. 5- F-55 [J]., 2014, (2): Li HA, Wu BL, Xu YM, et al. Research on the changes of 5-hydroxymethyl furfural during the F55-fructose syrup storage [J]. Food Eng, 2014, (2): [8],,, [J]., 2014, 35(17): Zhang YY, Zhang X, Zhang HY, et al. Kinetic studies on 5-hydroxymethylfurfural formation in 3 kinds of monosaccharide solution model system during thermal processing [J]. Food Sci, 2014, 35(17): [9] Lalou S, Hatzidimitriou E, Papadopoulou M. Beyond traditional balsamic vinegar: compositional and sensorial characteristics of industrial balsamic vinegars and regulatory requirements [J]. J Food Compos Anal, 2015, 43: [10],,,. 5- [J]. ( ), 2014, 77(3): Yi KY, Cao YX, Li JM, et al. Determination of 5-hydroxymethylfurfural in soy by the method of derivative spectrophotometry [J]. Chem, 2014, 77(3): [11],,,. [J]., 2014, 45(1): Zhou YQ, He FY, Yang YT, et al. Research situation of Maillard reaction and its influence on research methods for processing and preparation

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6 process of Chinese materia medica [J]. Chin Tradit Herbal Drugs, 2014, 45(1): [12],. [J]., 2005, 17(1): Zheng WH, Xu X. Research progress on Maillard reaction [J]. Prog Chem, 2005, 17(1): [13] Serra-Cayuela A, Castellari M, Bosch-Fust J, et al. Identification of 5-hydroxymethyl-2-furfural(5-HMF) in Cava sparkling wines by LC-DAD-MS/MS and NMR spectrometry [J]. Food Chem, 2013, 141: [14] Oral R A, Mortaș M, Doğan M, et al. New approaches to determination of HMF [J]. Food Chem, 2014, 143: [15] Anese M, Suman M. Mitigation strategies of furan and 5-hydroxymethylfurfural in food [J]. Food Res Int, 2013, 5l(1): [16] GB/T [S]. GB/T National food safety standard-honey [S]. [17] GB/T [S]. GB/T National food safety standard-apple juice concentrate [S]. [18] Kumar G, Sivagurunathan P, Kobayashi T, et al. Simultaneous removal of 5-hydroxymethylfurfural(5-HMF) and hydrogen production from acid(h 2 SO 4 ) pretreated red-algal hydrolysate via hybrid immobilized cells [J]. Algal Res, 2015, 11: [19], [J]., 2014, 33(1): Huang XW, Feng XJ. Determination of 5-hydroxymethyl furfural and furfural in caramel for soy sauce by SPE-HPLC [J]. China Brew, 2014, 33(1): [20],,, [J]., 2016, 37(2): Wang LL, Dong R, Fan C, et al. Changes in the contents of 5-HMF, 10-HDA and AFG in royal jelly during storage [J]. Food Sci, 2016, 37(2): [21],,,. 5- [J]., 2016, 17: Zhang L, Pan HH, Liu F, et al. Content variation of 5-hydroxymethylfurfural in bran-frying process of atractylodis macrocephalae rhizomaand its correlation with temperature and color changes of decoction pieces [J]. Chin J Exp Tradit Med Formul, 2016, 17: [22],,,. 40 ph 5- [J]., 2015, (10): Guo HY, Geng QG, Wang CH, et al. Correlation analysis of furfural, 5-hydroxymethylfurfural content and ph value of dextran 40 and glucose injection [J]. Chin J Pharmacov, 2015, 10: [23],,,. 5- [J]., 2014, 35(3): Zhang YY, Zhang X, Zhang HY, et al. Analysis of the formation kinetics on 5-hydroxymenthylfurfual in disaccharide system during thermal processing [J]. Sci Technol Food Ind, 2014, 35(3): [24],,,. [J]., 2016, (7): Zhang YY, Sun Y, Zhao J, et al. Sequential orthogonal optimization of thermal reaction technology for pork ribs soup flavoring [J]. Fine Chem, 2016, (7): [25]. [J]., 2015, (3): Gao YJ. Study on the optimization of preparation process of sweet and sour spareribs [J]. J Sichuan Tour Coll, 2015, (3): 作者简介 ( 责任编辑 : 刘丹 ) 张莉莉, 硕士研究生, 主要研究方向为食用香料化学及其应用 @qq.com 张玉玉, 博士, 副教授, 主要研究方向为食用香料化学及其应用 zhangyy2@163.com

Microsoft Word - 3098-3102 20150611007-蔡伟江-二校

Microsoft Word - 3098-3102 20150611007-蔡伟江-二校 6 8 Vol. 6 No. 8 2015 8 Journal of Food Safety and Quality Aug., 2015 蔡伟江 *, 邓鹏飞, 刘光兰, 李丹 (, 519040) 摘要 : 目的, 方法 (4.6 mm 250 mm, 5.0 μm) ; : : : =70: 16: 14(V:V:V),, : 1.0 ml/min; : 40 ; : 10

Microsoft Word 张莉莉_二校 出4023

Microsoft Word 张莉莉_二校出4023