Microsoft Word _李疆-二校

Size: px

Start display at page:

Download "Microsoft Word _李疆-二校"

祷宓
5 years ago
Views:

1 7 2 Vol. 7 No Journal of Food Safety and Quality Feb., 2016 李疆 1 1, 2,, 陈桐 3, 鞠昭函 4, 赵珊 1, 丁晓静 1, 3* (1.,, ; 2., ; 3., ; 4., ) 摘要 : 目的方法, 0.45 μm (50 µm 60.2 cm), 8 mmol/l 3, 5-10 mmol/l 0.5 mmol/l -20 kv, 200 nm, 结果 3.00 mg/l(s/n=3), mg/l (S/N=9), 10.00~300.0 mg/l, r mg/l, 103.2% 103.3% 104.8%, 0.5% 1.2% 0.7%(n=3) 结论, 11 min ( 6 min 5 min),, 关键词 : ; ; ; 3, 5- Determination of xylitol by capillary zone electrophoresis with indirect ultraviolet detection in food LI Jiang 1, CHEN Tong 1, 2, 3, JV Zhao-Han 4, ZHAO Shan 1, DING Xiao-Jing 1, 3 (1. Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning, Beijing Center for Disease Control and Prevention, Beijing , China; 2. Beijing Anzhen Hospital Affiliated to Capital Medical University, Beijing , China; 3. Department of Public Health, Capital Medical University, Beijing , China; 4. College of Arts and Science of Beijing Union University, Beijing , China) ABSTRACT: Objective To develop a new method for the detection of xylitol in food by capillary zone electrophoresis with indirect ultraviolet. Methods Samples were extracted with ultrapure water, centrifuged and injected by 0.45 μm membrane. The separation was carried out using an uncoated fused-silica capillary with 50 µm i.d. and 60.2 cm total length. The separation buffer consisted of 8 mmol/l 3, 5-dinitrobenzoic acid, 10 mmol/l sodium tetraborate and 0.5 mmol/l hexadecyl trimethyl ammonium bromide, separation voltage was -20 kv and the detection wavelength was 200 nm. Quantification was made by external calibration between the corrected peak area and the concentration of xylitol. Results The limit of detection and limit of quantitation were 3.00 mg/l (S/N=3) and mg/l (S/N=9), respectively. The linear range between the corrected peak area and the concentration was from to mg/l with a correlation coefficient of The average spiked recoveries of 3 levels (20.00, and mg/l) were 103.2, and 104.8% 基金项目 : ( ) Fund: Supported by the Beijing Municipal Health Bureau for the Project of Training High-level Medical Technical Personnel in Health System ( ) * 通讯作者 :,, dxj_wry@yahoo.com *Corresponding author: DING Xiao-Jing, Professor, Beijing Center for Disease Control and Prevention, No.16, Hepingli Middle Street, Dongcheng District, Beijing , China. dxj_wry@yahoo.com

2 792 7 with relative standard deviations of 0.5%, 1.2% and 0.7%, respectively. Conclusion The method is simple and fast and the analysis could be completed within 11 min (6 min for rinsing and 5 min for separation), which is suitable for the determination of xylitol in food samples. KEY WORDS: capillary zone electrophoresis; indirect ultraviolet detection; xylitol; 3, 5-dinitrobenzoic acid 1 引言, [1],, [2],, [3] [4],,,,,, [5],, (GC) [6],,,,, 12~24 h, [7],,, [8] [9] [10] [11] [12-15] [16] [17, 18] (IC), GC, HPLC, [10, 14-17] ; IC, 40 min,, -,, 2 材料与方法 2.1 仪器与试剂 P/ACE MDQ ( Beckman ); Millipore Milli-Elix/RiOs ( Millipore ); Universal 32 ( Hettich ); ( Gilson ); A11B S25 ( IKA ); F-50A ( ) 3, 5- (, ); (, ); NaOH(, ); (CTAB, Sigma-Aldrich, 99%); : (Chemservice, 99%); (USP ); (, 98%); (Sigma-Aldrich, 99%); (, 99%); (, 98%); (, ); ph ; 50 μm ( );, : 100 mg 15 ml, 10 ml, 10 mg/ml, 电泳条件 : 50 µm 60.2 cm ( : 50 cm), : 8 mmol/l 3, 5-, 10 mmol/l, 0.5 mmol/l CTAB; : -20 kv; : 200 nm; : 4 ; : 0.5 psi 20 s; : 10.3 μa 2.3 实验方法毛细管的预处理 1 mol/l NaOH 20

3 2, : min 5 min 5 min, 1 mol/l NaOH 2 min, 样品前处理 : 1 ml(, 0.1g ), 15 ml, 1 ml 50 mmol/l 10 ml, 0.45 μm, 1.5 ml :, 0.1 g, 50 mmol/l, 10 ml :, 0.1 g 15 ml, 10 ml, 15 min, 9000 r/min 10 min, 0.45 μm, 200 nm 3.3 探针浓度的选择, 3 ~10 mmol/l 3 mmol/l,,,,,, 8 mmol/l,, 8 mmol/l, 1 3 结果与分析 3.1 毛细管内径长度及进样时间的选择,, 50 µm, :, 60.2 cm, 50 µm 60.2 cm( : 50 cm) CE Expert 20 s ( min) :,, 20 s, 3.2 探针及检测波长的选择,,, ( ), [19], [20] [21], 3, nm,, 1 3, 5- Fig. 1 Effects of the concentration of 3, 5-dinitrobenzoic acid on the separation of xylitol 1 ; 2 1. xylitol; 2.unknown 3, 5- (mmol/l): a. 3; b. 8; c. 10 3, 5-dinitrobenzoic acid(mmol/l): : a. 3; b. 8; c 分离缓冲体系及其浓度的选择,, [22] -, [23], 10 mmol/l [24]

4 mmol/l,,,,, 10 mmol/l, ~300.0 mg/l, 3.00 mg/l(s/n=3), mg/l(s/n = 9) mg/l 7, (RSD) RSD 0.70% 0.50% 1.1%; RSD 2.0% 0.79% 0.71% ,, RSD 3.4 % 3.7 回收率试验, 2.3.2, mg/l 3, 3 3, 1 Fig. 2 2 Effects of the concentration of sodium borate on the separation of xylitol 1 ; 2 1 xylitol; 2 unknown (mmol/l): a. 10; b. 12; c. 15 Concentration of sodium borate: a. 10 mmol/l b. 12 mmol/l c. 15 mmol/l. 3.5 电渗流改性剂浓度的选择, EOF, (30 min), CTAB EOF, [25] : 0.5 mmol/l CTAB EOF, 0.5 mmol/l CTAB EOF 3.6 工作曲线线性范围检出限和精密度 mg/l,, ( ) (x, mg/l), A=17.14 x+25.83, r=0.9994, 3 Fig. 3 Electrophoregrams of spiked blank sample a. 80 mg/l ; b. ; c. 80 mg/l a. 80 mg/l xylitol standard; b. blank sample; c. blank sample spiked with 80 mg/l xylitol standard 表 1 木糖醇 3 水平加标回收率结果 (n=3) Table 1 The recoveries of xylitol at 3 spiked levels(n=3) /(mg/l) /% RSD/%

5 2, : 样品分析 5 6,, 2, 4 表 2 食品中木糖醇的测定结果 (n=5) Table 2 The content of xylitol in foods (n=5) /(g/kg) RSD% 干扰实验 1000 mg/l ( ) 500 mg/l ( ),, 4 结论 -,, 11 min,,,, 参考文献 [1],. [J]., 2011, 36(3): Liu T, Wu DC. Analytical methodologies for determination of sweeteners in foodstuffs [J]. China Condiment, 2011, 36(3): [2]. [J]., 2008, 2: Wang R. Functional sweetener xylitol and application in food processing [J]. Jiangsu Food Fermen, 2: [3],,,. [J]., 2001, 19 (6): Chen GH, Zhang LP, Tian YL, et al. Separation of xylose and xylitol in fermentation liquid by capillary zone electrophoresis [J]. Chin J Chromatogr, 2001, 19(6): [4] GB [S]. GB National Food Safety standards Standards for uses of food additives [S]. [5],,,. HPLC-ELSD 10 [J]., 2013, 34(12): Lin H, Yan CR, Xu CX, et al. Simultaneous determination by 4 Fig. 4 Electrophoregrams of clinical nutrition powder sample and chewing gum sample 1 a. 50 mg/l ; b. ; c. 1 xylitol a. 50 mg/l xylitol standard; b. clinical nutrition powder sample; c. chewing gum sample HPLC-ELSD of ten kinds of sugars and sugar alcohols in food [J]. Food Sci, 2013, 34(12): [6],,,. [J]., 2000, 11(5): Cao YL, Liu HL, Li YL, et al. Gas chromatography determination xylitol in the food [J]. Henan J Prev Med, 2000, 11(5):

6 796 7 [7],,. [J]., 2005, 3: Wang CF, Zhao GH, Zhou J. Determines xylitol by capillary column GC [J]. Chin Food Addi, 2005, 3: [8],,,. - [J]., 2014, 33(9): Liu YP, Chen LY, Zhang J, et al. Simultaneous determination of glucose and six sugar alcohols in foods by capillary electrophoresis with ultra-violet detection [J]. Chin J Anal Lab, 2014, 33(9): [9],,,. - [J]., 2010, 3: Yu C, Yan Z, Cai LP, et al. Determination of content of alditol in sugar-free cakes by high performance liquid chromatographyevaporative light scattering detector (HPLC-ELSD) [J]. Sci Technol Food Ind, 2010, 3: [10],,,. HPLC [J]. ( ), 2005, 26(1): 61 62, 67. Shi 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 (Nat Sci Edi), 2005, 26(1): 61 62, 67. [11] Grembecka M, Lebiedzińska A, Szefer P. Simultaneous separation and determination of erythritol, xylitol, sorbitol, mannitol, maltitol, fructose, glucose, sucrose and maltose in food products by high performance liquid chromatography coupled to charged aerosol detector [J]. Microchem J, 2014, 117(6): [12] Nojiri S, Taguchi N, Oishi M, et al. Determination of sugar alcohols in confectioneries by high-performance liquid chromatography after nitrobenzoylation [J]. J Chromatogr A, 2000, 893: [13],,,. [J]., 2007, 28(6): Li L, Liu YF, Tang HD, et al. Determination of sugar alcohol in foods by HPLC method [J]. Food Sci, 2007, 28(6): [14],,,. [J]., 2002, 1(4): Qin ZS, Wang P, Chen GR, et al. Determination of xylitol by high performance liquid chromatography [J]. Chin J Public Health Eng, 2002, 1(4): [15] Hanko VP, Jeffrey SR. 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: [16],,. [J]., 2007, 35(11): Bai JG, Song LH, Zhou WH. Determination of xylitol and sorbitol in sugar free chewing gums by miniaturized capillary electrophoresis system with amperometric detection [J]. Anal Chem, 2007, 35(11): [17],,,. - [J]., 2013, 31(11): Zhou HB, Xiong ZY, Li P, et al. Determination of alditols in foods by ion chromatog raphy-mass spectrometry [J]. Chin J Chromatogr, 2013, 31(11): [18],,,. - 3 [J]., 2013, 4(1): Zeng SD, Du HQ, Guo HB, et al. Determination of three synthetic sweeteners in fruits by ultra pressure liquid chromatography-mass spectrometry [J]. J Food Saf Qual, 2013, 4(1): [19] Johns C, Macka M, Haddad PR. Enhancement of detection sensitivity for indirect photometric detection of anions and cations in capillary electrophoresis [J]. Electrophoresis, 2003, 24: [20]. [M]. :, Chen Y. Capillary electrophoresis technology and application [M]. Beijing: Chemical Industry Press, [21],,,. - [J]., 2014, 32 (6): Chen T, Ding XJ, Li LZ, et al. Rapid determination of cyclamate in food by capillary zone electrophoresis with indirect ultraviolet detection [J]. Chin J Chromatogr, 2014, 32 (6): [22],. [J]., 2001, 19 (4): Mao XL, Lin BC. Capillary electrophoresis and chip capillary electrophoresis of carbohydrate [J]. Chin J Chromatogr, 2001, 19 (4): [23] Mccourt J, Stroka J, Anklam E. Experimental design-based development and single laboratory validation of a capillary zone electrophoresis method for the determination of the artificial

2, : - 797 sweetener sucralose in food matrices [J].

Indirect photometric detection in CE using buffered electrolytes-part I, principles [J].

Determination of thioglycolic acid in cosmetics by capillary electrophoresis [J].

7 2, : sweetener sucralose in food matrices [J]. Anal Bioanal Chem, 2005, 382(5): [24] Macka M, Johns C, Philip DA, et al. Indirect photometric detection in CE using buffered electrolytes-part I, principles [J]. LC GC North Am, 2001, 19(1): [25] Xie N, Ding X, Wang X, et al. Determination of thioglycolic acid in cosmetics by capillary electrophoresis [J]. J Pharm Biomed, 2014, (88): ( 责任编辑 : 金延秋 ) 作者简介李疆, 副主任技师, 主要研究方向为食品加工及食品安全分析 lij0993@sohu.com 丁晓静, 主任技师, 主要研究方向为色谱技术在卫生检验中的应用 dxj_wry@yahoo.com

g ml 10% ph 色谱条件 kinetex C μm 100 A 4. 6 mm 150 mm 25 5 μl A B 10 mmol /L ml /min

g ml 10% ph 色谱条件 kinetex C μm 100 A 4. 6 mm 150 mm 25 5 μl A B 10 mmol /L ml /min 25 4 2013 8 监测技术 5 1 2 1 ( 1. 江苏省疾病预防控制中心, 江苏南京 210009; 2. 南京医科大学第二附属医院, 江苏南京 210029) 5 Phenomenex kinetex C 18 2. 6 μm 4. 6 mm 150 mm 10 mmol /L ph 2. 5 + 60 40 DAD 280 nm 5 20. 0 mg /L ~ 100 mg /L 0.