Microsoft Word 陈树东-二校

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1 7 5 Vol. 7 No Journal of Food Safety and Quality May, 陈树东 *, 林晓佳, 林森煜, 刘海虹, 严婉盈, 吴钟玲 (, ( ), ) 摘要 : 目的 - (HPLC-RID), 7 方法 Phenomenex HPX-42C,,, 结果 7 (Van t Hoff), ; 50~0 mg/l, (r 2 )0.999, 25 mg/kg, 94.4%~108%, 0.95%~7.3% 结论, 关键词 : ; ; Simultaneous detection of 7 kinds of sugar alcohols in the gum base candy by high performance liquid chromatography CHEN Shu-Dong *, LIN Xiao-Jia, LIN Sen-Yu, LIU Hai-Hong, YAN Wan-Ying, WU Zhong-Ling (Guangzhou Quality Supervision and Testing Institute, National Centre for Quality Supervision and Testing of Processed Food (Guangzhou), Guangzhou , China) ABSTRACT: Objective To develop a high performance liquid chromatography with refractive index detection (HPLC-RID) method for the simultaneous determination of maltitol, ribitol, glycerine, mannito, lactitol, xylitol and sorbitol in gum based candy. Effects of temperature and flow rate on the separation efficiency of 7 kinds of sugar alcohols were investigated and optimized. Methods Using Phenomenex HPX-42C column with refractive index detector, ultra pure water as mobile phase, the content of sugar alcohols were determined by external standard method. Results The Van't Hoff curves of 7 kinds of sugar alcohols under different temperature conditions had good linear relationships. The separation effect of different sugar alcohols could be improved by changing the column temperature. It showed good linear relationships in the range of 50~0 mg/l, and the limits of quantitation (LOQ) of 7 kinds of sugar alcohols were 25 mg/kg, respectively. The recoveries were 94.4%~108.5% and the relative standard deviations were 0.95%~7.34%. Conclusion The method is simple with good separation effect, and is suitable for the detection of sugar alcohols in gum based candy. KEY WORDS: sugar alcohol; gum base candy; high performance liquid chromatography * 通讯作者 :,, uu3g@163.com *Corresponding author: CHEN Shu-Dong, Engineer, Guangzhou Quality Supervision and Testing Institute, No.1-2 Zhujiang Road, Chaotian Industrial District, Panyu District, Guangzhou , China. uu3g@163.com

(r 2 )0.999, 25 mg/kg, 94.4%~108%, 0.95%~7.

2 5, : 引言,, [1] (sugar alcohol),,,, 50% (-CHO >C=O) (-OH) (polyols), ( ), ( ) [2],, [3],,,,, : (HPLC) [4-8] [9-12] (GC) [13-15] -(GC-MS) [16,17] - (LC-MS/MS) [18],,,, GC [13,14] ;,, [9,10],,,, [4],, (HPLC-RID) (HPLC-ELSD) [5-8],,,, 3, [1,4-8],,,,,,, 7 ( 3 ), 2 材料与方法 2.1 仪器与设备 1260 (HPLC), ( Agilent ); IKA ( IKA ); MS3 basic ( IKA ); KDC-400 ( ); KQ-E ( ); Milli-Q ( Millipore ); Phenomenex HPX 42 C (300 mm 7.8 mm); Zorbax (250 mm 4.6 mm, 5 μm) 2.2 标准品与试剂 ( Sigma, 98%) ( Sigma, 98%) ( Fluka, 99.5%) ( Dr. Ehrenstorfer, 99.5%) ( Aladdin, 99%) ( Dr. Ehrenstorfer, 99%) ( Dr. Ehrenstorfer, 99%)(Merck) (18.2 MΩ) 2.3 标准溶液配制 7 : 0.1 g( 0.1mg), 10 ml, 00 mg/l 4 7 :, 前处理, IKA, 2.0 g 50 ml, 30 ml,, 5 min, 4000 r/min 2 min, ml ; 30 ml, 3,, 0.22 μm 2.5 仪器条件 (HPLC): : Phenomenex HPX 42 C ; : ; : 0.50 ml/min; : 50 ; : (RID); : 50 3 结果与分析 3.1 色谱柱的选择, Zorbax, - (85:15, V:V), 1.0 ml/min 7, 1,,,,,,,

1 仪器与设备 1260 (HPLC), ( Agilent ); IKA ( IKA ); MS3 basic ( IKA ); KDC-400 ( ); KQ-E ( ); Milli-Q ( Millipore ); Phenomenex HPX 42 C (300 mm 7.8 mm); Zorbax (250 mm 4.6 mm, 5 μm) 2.

3 1910 7,,,, ( ),, 7, 7, [19],,, 7,,,,, ;, 旳, [20], - HPX 42 C (7.8 mm 30 mm) 7, 2,,,, 1 Zorbax 7 Fig. 1 Separation chromatogram of Zorbax NH 2 column 2 HPX 42 C 7 Fig. 2 Separation chromatogram of Ca 2+ ion exchange column of Phenomenex HPX 42 C

4 5, : 色谱柱柱温的影响,,, ,, (Van t Hoff) : H S lnk = ln, k RT R, T, ΔH ΔS, R, φ ΔH ΔS lnk (1/T) lnk 1/T, -ΔH/R, ;,,, 3 7, 1, 7, 7 [21], 7,, 7 ( 3),,,,,, 50 7, 流动相流速的确定,,,,,,,, ml/min,, 0.5 ml/min, 7, 30 min, 0.5 ml/min 3.4 线性关系与检出限 7, Y, X(mg/L),, S/N = 3, 7 (LOD), 2, 7, 0.999, 25 mg/kg 3.5 方法的精密度和回收率, 3 7,,, 6, (RSD), 3,, %~108.5%, (RSD, n=6) 0.95%~7.34%, Fig The Van t Hoff plots of 7 kinds of sugar alcohols at different temperatures

1, 7, 7 [21], 7,, 7 ( 3),,,,,, 50 7, 50 3.3 流动相流速的确定,,,,,,,, 0.30 0.40 0.50 0.60 0.65 0.70 0.75 0.80 ml/min,, 0.

5 表 1 7 种糖醇范特霍夫 (Van t Hoff) 曲线回归数据 Table 1 Linear regression data for plot of lnk vs 1/T of sugar alcohols ΔH/R, ΔS/R + lnφ, r 2 1 (lactitol) (maltitol) (ribitol) (glycerine) (mannitol) (xylitol) (sorbitol) 表 2 标准曲线及检出限 Table 2 Calibration curves and detection limits (mg/l) (mg/l) 1 (lactitol) Y = X ~ (maltitol) Y = X ~ (ribitol) Y = X ~ (glycerine) Y = X ~ (mannitol) Y = X ~ (xylitol) Y = 293.7X ~ (sorbitol) Y = X ~ Table 3 表 3 7 种糖醇的相对标准偏差和回收率 (n=6) Relative standard deviations and recoveries of 7 kinds of sugar alcohols (n=6). (mg/kg) (%) (%) 1 (lactitol) 2 (maltitol) (ribitol) (glycerine) 5 (mannitol) (xylitol) (sorbitol) 样品测定 10 7, 4, ( ),, 50%,,

9993 表 2 标准曲线及检出限 Table 2 Calibration curves and detection limits (mg/l) (mg/l) 1 (lactitol) Y = 290.14 X 3343.3 50~0 0.9998 25 2 (maltitol) Y = 296.93X 4006.8 50~0 0.

6 5, : (g/ g) 表 4 10 种胶基糖果中糖醇的检测结果 Table 4 Contents of sugar alcohols in gum based candy (g/ g) (g/ g) (g/ g) (g/ g) (g/ g) (g/ g) 1 ND ND ND 0.19 ND ND ND 2 ND ND ND 0.17 ND ND ND 3 ND ND ND 0.25 ND ND ND 4 ND ND ND 1.20 ND ND ND 5 ND 2.24 ND ND 2.31 ND ND ND ND ND 2.38 ND ND 0.39 ND ND ND ND : ND 4 结论 RID 7,,,, 参考文献 [1] GB/T [S]. GB/T Determination of xylitol sorbitol maltitol in foods-high-performance liquid chromatography [S]. [2]. [M]. :, You X. Production and application of starch sugar handbook [M]. Beijing: China Light Industry Press, [3] SN/T : [S]. SN/T Rules for the inspection of food additives for import and export. Part 8: Chewing gum bases and ingredients [S]. [4] Medeiros PM, Simoneit BRT. Analysis of sugars in environmental samples by gas chromatography mass spectrometry [J]. J Chromatogr A, 2007, 1141(2): [5] Bhandari P, Kumar N, Singh B, et al. Simultaneous determination of sugars and picrosides in Picrorhiza, species using ultrasonic extraction and high-performance liquid chromatography with evaporative light scattering detection [J]. J Chromatogr A, 2008, 1194(2): [6] Liu XJ, Ai N, Zhang HY, et al. Quantification of glucose, xylose, arabinose, furfural, and HMF in corncob hydrolysate by HPLC-PDA ELSD [J]. Carbohyd Res, 2012, 353(9): [7],,,. - [J]., 2009, (B12): Shi HL, Yang HM, Wang H, et al. Determination of sugar alcohol in no sugar foods by HPLC method [J]. Anal Lab, 2009, 2: [8],,,. HPLC [J]. :, 2005, 26(1): Si YZ, Guo XQ, Yu QR, et al. Determination of many kinds of components in chewing gum by HPLC with refractive index detector [J]. J Capital Normal Univ (Sci Ed), 2005, 26(1): [9],. -[J]., 2005, 33(4): Ding YS, Mou SF. Application of high performance anion exchange chromatography with pulsed electrochemical detection [J]. Chin J Anal Chem, 2005, 33(4): [10] Hanko VP, Rohrer JS. Determination of carbohydrates, sugar alcohols, and glycols in cell cultures and fermentation broths using high-performance anion-exchange chromatography with pulsed amperometric detection [J]. Anal Biochem, 2000, 283(2): [11],,,. -[J]., 2009, 29(6): Tang KT, Lin L, Liang LN, et al. Simultaneous determination of sugars and sugar alcohols in sugar-free and low-sugar food with high performance anion-exchange using pulsed amperometric detection [J]. Food Sci, 2009, 29(6): [12],,. [J]., 2010, 28(4):

41 9 ND 0.39 ND 1.89 4.89 38.80 28.93 10 ND ND ND 1.64 4.89 42.20 32.43 : ND 4 结论 RID 7,,,, 参考文献 [1] GB/T 22222-2008.

7 Liu YF, Tang HC, Li D. Determination of sugars and sugar alcohols in foods by ion exchange chromatography [J]. J Beijing T & B Univ, [13] Adams MA, Chen ZL, Landman P, et al. Simultaneous determination by capillary gas chromatography of organic acids, sugars, and sugar alcohols in plant tissue extracts as their trimethylsilyl derivatives [J]. Anal Biochem, 1999, 266(1): [14],,. [J]., 2005, (3): Wang CF, Zhao GH, Zhou J. Determ ines xylitol by capilary column GC [J]. China Food Addit, 2005, (3): [15] Bartolozzi F, Bertazza G, Bassi D, et al. Simultaneous determination of soluble sugars and organic acids as their trimethylsilyl derivatives in apricot fruits by gas-liquid chromatography [J]. J Chromatogr A, 1997, 758(1): [16] Tetsuo M, Zhang C, Matsumoto H, et al. Gas chromatographic mass spectrometric analysis of urinary sugar and sugar alcohols during pregnancy [J]. J Chromatogr B, 1999, 731(1): [17] Katona ZF, Sass P, Molnár-Perl I. Simultaneous determination of sugars, sugar alcohols, acids and amino acids in apricots by gas chromatography mass spectrometry [J]. J Chromatogr A, 1999, 847(1): [18] Cheng C, Tsai HR, Chang KC. On-line cut-off technique and organic modifier addition aided signal enhancement for trace analysis of carbohydrates in cellulase hydrolysate by ion exclusion chromatographyelectrospray ionization mass spectrometry [J]. J Chromatogr A, 2006, 1119(1 2): [19] Hao H, Hou B, Wang JK, et al. Effect of solvent on crystallization behavior of xylitol [J]. J Cryst Growth, 2006, 290(1): [20],. [J]., 2007, 9(1): Liu XL,Shu J. Discussion on the treatment technology of ion exchange resin [J]. J Liaoning Univ TCM, 2007, 9(1): [21] Yu H, Li R. Effect of column temperature on the retention of inorganic anions and organic acids in non-suppressed anion-exchange IC [J]. Chromatographia, 2008, 68(7 8): 作者简介 ( 责任编辑 : 金延秋 ) 陈树东, 工程师, 主要研究方向为食品和农产品质量安全检测技术 uu3g@163.com

Anal Biochem, 1999, 266(1): 77 84. [14],,. [J]., 2005, (3):104 107. Wang CF, Zhao GH, Zhou J. Determ ines xylitol by capilary column GC [J]. China Food Addit, 2005, (3): 104 107.

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