Microsoft Word 刁飞燕-二校938

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1 7 3 Vol. 7 No Journal of Food Safety and Quality Mar., 2016 C * 刁飞燕, 刘春霖, 吴晓云, 李启艳 (, ) 摘要 : 目的 C 方法 CAPCELL PAK NH 2 (4.6 mm 250 mm, 5 μm), - (70:30, V:V), 1 ml/min, 35, 结果 10.50~ µg (r=0.9993) 9.98~99.72 µg (r=0.9999) 9.72~97.24 µg (r=0.9980), 2 µg; 95.1% 92.7% 92.6%, RSD 1.56% 2.22% 1.76% 结论,, C 关键词 : ; C ; ; ; Determination of xylitol, sorbitol and sucrose in chewable and effervescent vitamin C by high performance liquid chromatography DIAO Fei-Yan, LIU Chun-Lin, WU Xiao-Yun, LI Qi-Yan * (Shandong Institute for Food and Drug Control, Jinan , China) ABSTRACT: Objective To establish a method for the determination of xylitol, sorbitol and sucrose in chewable and effervescent vitamin C by high performance liquid chromatography. Methods Samples were separated on a CAPCELL PAK NH 2 column (4.6 mm 250 mm, 5 µm). The mobile phase consisted of water and acetonitrile (30:70, V:V). The flow rate was 1.0 ml/min, column temperature was 35, and samples were detected with refractive index detector. Results The standard curve of xylitol was linear over the range in 10.50~ µg (r=0.9993). The standard curve of sorbitol was linear over the range in 9.98~99.72 µg (r=0.9999). The standard curve of sucrose was linear over the range in 9.72~97.24 µg (r=0.9980). The limit of detection was 2 µg. The recovery was 95.1%, 92.7% and 92.6% and the RSD was 1.56%, 2.22% and 1.76%, respectively. Conclusion Each substance can be separated with this method, which is simple, rapid and accurate. It can be used for the determination of xylitol, sorbitol and sucrose in chewable and effervescent vitamin C. KEY WORDS: high performance liquid chromatography; chewable and effervescent vitamin C; xylitol; sorbitol; sucrose * 通讯作者 :,, @163.com *Corresponding author: LI Qi-Yan, Deputy Chief Pharmacist, Shandong Institute for Food and Drug Control, No. 2749, the New Lok Street, High-tech District, Jinan , China @163.com

2 3, : C 引言 C,, C,, C C, C, [1],, [2] [3] [4] [5] [6-15],,, (high performance liquid chromatography, HPLC) 3,, 2 材料与方法 2.1 材料与试剂 C (4 ), C (9 ) EC EC (, : ); C (, : ); C (, : ); C (, : ); C (, : ); C (, : ) (, Merker ); ( Millipore ); ( 99.0%, Dr Ehrenstorfer GmbH, : 80826); ( : , ); ( 99.8%, : , ) 2.2 仪器与设备 MettlerToledo MS ( - ); Waters e2695 ( Waters 2414, Waters ); KQ-500DE ( ); TDZ5-WS ( ); FW-100 ( ); BPZ-6063 ( ) 2.3 实验方法色谱条件 : CAPCELL PAK NH 2 (4.6 mm 250 mm, 5 μm); : 35 ; : : (70:30, V:V); : 1 ml/min; : ( 35 ) : 20 μl 溶液的配制 (1) 10 ml, 10 mg/ml, mg/ml (2), 50 ml, 40 ml, 20 min,,, 3500 r/min 5 min, 0.45 µm, HPLC (3), C,, 2.3.2(2), 3 结果与分析 3.1 检测器和色谱柱的选择,, 3,,,, Prevail Carbohydrate ES, CAPCELL PAK NH 2,,

3 样品提取方法与试剂的选择 3, 1,,,,,,, ; 2, 30 min,,,, ; 3, 70% 30 min,,,,, 3, 1,,, ; 3,,, 2, 3.3 标准与样品图谱 µl,,,,,,,, 1~ 4 Fig. 1 1 (1- ; 2- ; 3- ) Chromatogram of standard sample (1-xylitol; 2-sorbitol; 3-sucrose) 2 (2- ) Fig. 2 Chromatogram of chewable tablets (2-sorbitol)

4 3, : C 941 Fig.3 3 (3- ) Chromatogram of effervescent tablets (3-sucrose) Fig. 4 4 Chromatogram of blank samples 3.4 标准曲线与检出限, 2.3.1, (X), (Y), : Y= X , r=0.9993, : 10.50~ µg; Y= X , r=0.9999, : 9.98~99.72 µg; Y= X , r=0.9980, 9.72~97.24 µg 3, 2 µg 3.5 仪器精密度实验 2 mg/ml 5, RSD 1.56% 1.19% 1.98%, 3.6 方法精密度和回收率实验 2.3.2(3) 5, 50 mg, 2.3.2(2),, 1

5 942 7 Table 1 表 1 各检测物质回收率 Recoveries and relative standard deviations (mg) (mg) (%) (%) RSD (%) ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND : ND ; RSD: 3.7 样品的测定 13 (4, 9 ), 2.3.2(2), 2 表 2 样品测定结果 (n=3) Table 2 Results in sample for all three substances (n=3) (g/100 g) (g/100 g) (g/100 g) 1 ND ND ND ND ND ND ND ND ND ND ND 9 ND ND ND ND ND ND 12 ND ND 13 ND ND : ND, 1-9, , 13, 1 3, 6, 2, 3, 1, 5.75~48.90 g/100 g, 2.09~36.75 g/100 g 4 讨论 C,, 5.75~48.90 g/100 g, 2.09~36.75 g/100 g,,,,,,, C, 参考文献 [1] U.S. Food and Drug Administration. A food labeling guide [S].

6 3, : C 943 [2],,. HPLC C [J]., 2004, 1: Ding JH, Rao HY, Wang XX. Study of the factors which affect the stability of vitamic C by HPLC [J]. Food Ind, 2004, 1: [3] GB/T [S]. GB/T Reducing sugar determination in foods [S]. [4] GB/T [S]. GB/T Glucose determination in foods [S]. [5],,. [J]., 2003, 24(12): Fu CG, Shan RF, Su CH. Simultaneous determination on sucrose glucose and fructose in jujube by capillary electrophoresis with electrochemical detection [J]. Food Sci, 2003, 24(12): [6] GB/T [S]. GB/T Determination of saccharose in foods [S]. [7] Li J, Chen ML, Zhu Y. Separation an determination of carbohydrates in drinks by ion chromatography with a self-regenerating suppressor and an evaporative light-scattering detector [J]. J Chromatogr A, 2007, 1155: [8],,. [J]., 2009, (5): Diao CX, Zhang XM, Liu B. Improvement of determination method of the total sugar in dry red wine [J]. China Brew, 2009, (5): [9],,,. HPLC-ELSD 10 [J]., 2013, 34(12): Lin H, Yang CR, Xu CX, et al. Simultaneous determination by HPLC-ELSD of 10 kinds of sugars and sugar alcohols in foods [J]. Food Sci, 2013, 34(12): [10],,,. HPLC C C [J]., 2015, 25(10): Zhang J, Zhai ZL, Zhang W, et al. Simultaneous determination of vitamin C and sugar in chewable vitamin C by HPLC [J]. Chin J Health Lab Technol, 2015, 25(10): [11],,,. - [J]., 2014, 45(5): Liu YL, Ran XQ, Chen LY, et al. Simultaneous determination of sugar alcohols and sugars in functional foods by precolumn ultaviolet derivatization-high performance liquid chromatography [J]. J Sichuan Univ, 2014, 45(5): [12],,. [J]., 2015, 6(5): Chen XX, You JS, Yang ZW. Determination of sucralose content in health food by high performance liquid chromatography [J]. J Food Saf Qual, 2015, 6(5): [13],,. 4 [J]., 2014, 19(3): Huang R, Wu GB, Chen FH. Measurement of 4 common sugars and sugar alcohol in fruits by high performance liquid chromatography [J]. J Jimei Univ, 2014, 19(3): [14],, [J]., 2015, 6(10): Zhao WH, Zeng C, Cong YY. Determination of fructose, glucose, sucrose, and maltose in honey by high performance liquid chromatography with refractive index detector [J]. J Food Saf Qual, 2015, 6(10): [15],,,. - [J]., 2015, 6(2): Xu LZ, Li XY, Huang JF, et al. Simultaneous determination of monosaccharides, disaccharides and fructo-oligosaccharides in milk powder by ultra-filtration clean up coupled with HPLC [J]. J Food Saf Qual, 2015, 6(2): 作者简介 ( 责任编辑 : 杨翠娜 ) 刁飞燕, 主管药师, 主要研究方向为保健食品检测 @qq.com 李启艳, 副主任药师, 主要研究方向为保健食品质量控制 @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