Microsoft Word 蔡明明.doc

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1 5 7 Vol. 5 No Journal of Food Safety and Quality Jul., 2014 蔡明明 1, 陈启 1, 李爽 1, 任一平 (1., ; 2., ) 2* 摘要 : 目的方法 CarboPac PA20(3 mm 150 mm),, 结果, 0.2~20 mg/l, 0.999; ( 3) 10 mg/kg, ( 10) 30 mg/kg; 0.72%~1.53% 结论,,, 关键词 : ; ; Determination of lactose in human milk by ion chromatography CAI Ming-Ming 1, CHEN Qi 1, LI Shuang 1, REN Yi-Ping 2* (1. Beingmate Baby & Child Food Co., Ltd, Hangzhou , China; 2. Zhejiang Provincial Center for Disease Prevention and Control, Hangzhou , China) ABSTRACT: Objective To establish an analysis method by ion chromatography for the determination of lactose in human milk. Methods The modified gradient procedure was used to separate the lactose standard on a CarboPac PA20 (3 mm 150 mm) anion exchange column which was established automatic analysis method and used ion chromatography and external standard methods for quantitative analysis. Results Under optimal experimental condition, the lactose linear range of 0.2~20 mg/l, the correlation coefficient was greater than The method detection limit (S/N=3) was 10 mg/kg, the quantitative limit (S/N=10) was 30 mg/kg; lactose of human milk value was 0.72%~1.53%. Conclusion After method optimization, excluding impurities interference, lactose was determined more accurately. This method operation is simple, accurate and cheap, suitable for lactose in human milk analysis of the test. KEY WORDS: ion chromatography; human milk; lactose 1 引言,, [1],,,,,, [2], : [3], * 通讯作者 :,,, [email protected] *Corresponding author: REN Yi-Ping, Senior Engineer, Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou , China. [email protected]

2 7, : 2055,, (GC) [4,5] (HPLC) [6-9] (TLC) [10,11] (CE) [12] (IC) [13,14],, [15],, [16],,,,, 2 实验部分 2.1 仪器试剂与材料 : (Dionex ICS 5000,, ); ( Millipore ); (FOSS, ) (SHA-B, ); (SK8210HP, ); (Allegra 64R, Beckman ); (BSA224S-CW, Sartorius ) : ( 99.5% ) Sigma-Aldrich ; Sigma-Aldrich : OnGuard RP Dionex, : OnGuard II RP (2.5 cc) 10 ml 15 ml 30 min 2.2 标准溶液与淋洗液的配制 10 mg( 0.01 mg) 50 ml,, 200 mg/l, 4,, 1; (250 mmol/l): 13.1 ml 50%, 1000 ml; (500 mmol/l): 20.5 g,, 2.6 ml 50%, 500 ml; 18.2 MΩ.cm 1 Fig. 1 Chromatogram of lactose standard 2.3 仪器工作条件 : : CarboPac PA20(3 mm 150 mm); PG20(3 mm 30 mm); :, Au, Ag/AgCl ; : 30 ; : 0.45 ml/min; : 10 µl; : A: ; B: 250 mmol/l ; C: 500 mmol/l ; : 人乳取样方法来源保存条件表 1 梯度洗脱条件 Table 1 Eluent gradient for HPAEC PAD analysis (min) A B C 0 80% 20% 0% % 20% 0% % 10% 80% % 10% 80% % 80% 0% % 80% 0% % 20% 0% % 20% 0% 5

3 2056 5,,,, 样品预处理 0.5 g( 0.1 mg) 100 ml, 80 ml,, 3 ml 50%, 100 ml, 30 ml 50 ml ;, 1 ml 50 ml, 50 ml 15 ml, OnGuard RP, 7 ml,, 0.22 μm, CarboPac PA20 CarboPac PA10, CarboPac PA20 CarboPac PA10 OH - CarboPac PA20,, CarboPac PA20 2 CarboPac PA20 CarboPac PA10, 2 CarboPac PA20,,, CarboPac PA 红外光谱人乳成分分析仪法 76, FOSS 3 结果与讨论 3.1 人乳样品提纯净化,,,,,,,,,, 20% 30% 50% 55%,,, 50%, 50%, OnGuard RP, OnGuard RP 3.2 色谱分析柱的选择, pka 11~13, ph,,, Fig. 2 2 Comparison of chromatograms with different columns,,, 3, 3 Fig. 3 3 Chromatograms of human milk before and after digestion 3.3 方法学验证线性范围和检出限 mg/l,,,,

4 7, : 2057,,, 0.2~20 mg/l, 0.999, 2,, 1:3, 1:10, 精密度和回收率,, 6,,, 3, 99.53%~102.40%, 0.72%~ 1.53%,,, 人乳成分分析仪与离子色谱法比较实际样品测定结果 76,,,,,, 4, 6.70 g/100 g, 7.02%, 7.50 g/100 g, 5.20 g/100 g; 6.61 g/100 g, 4.99%, 7.37 g/100 g, 5.40 g/100 g,,, 4 结论,, : CarboPac PA20,, 76 :,,,, Table 2 表 2 乳糖的线性范围标准曲线相关系数检出限和定量限 Linearity range, standard curve, correlation coefficient, limits of detection(lod) and limits of quantitation(loq) of lactose (mg/l) (mg/kg) (mg/kg) 0.2~20 y=0.9693x Table 3 表 3 乳糖的加标回收率和相对标准偏差 (n=6) Recoveries and relative standard deviation of lactose(n=6) 3 g/100 g 6 g/100 g 9 g/100 g Table 4 表 4 不同人乳检测方法结果比较 Comparison of results with different methods

2058 5 参考文献 [1]. [M]. :, 2001. Wang GC. Food Nutrition[M]. Beijing: China Agriculture Press, 2001. [2],. [J]., 2000, 12(4): 13 15. Chen WC, Feng JJ.

Application of chromatography in analysis of carbohydrates[j]. Chin J Anal Chem, 2001, 29(2): 222 227. [4] Zhang W, He H, Zhang X.

5 参考文献 [1]. [M]. :, Wang GC. Food Nutrition[M]. Beijing: China Agriculture Press, [2],. [J]., 2000, 12(4): Chen WC, Feng JJ. Progress of glycoprotein oligosaccharides and monosaccharides chromatographic analysis[j]. Tianjin Pharmacy, 2000, 12(4): [3],. [J]., 2001, 29(2): Wang J, Wang Q. Application of chromatography in analysis of carbohydrates[j]. Chin J Anal Chem, 2001, 29(2): [4] Zhang W, He H, Zhang X. Determination of neutral sugars in soil by capillary gas chromatography after derivatization to aldononitrile acetates[j]. Soil Bio Biochem, 2007, 39(10): [5],,,. [J]., 2008, 39(4): Zhang W, He HB, Zhang M, et al. Determination of soil nitrile hydrolysis monosaccharide sugars derived acetyl esters by Gas Chromatography[J]. Chin J Soil Sci, 2008, 39(4): [6] Filson PB, Dawson-Andoh BE. Characterization of sugars from model and enzyme-mediated pulp hydrolyzates using high-performance liquid chromatography coupled to evaporative light scattering detection[j]. Bioresource Technol, 2009, 100(24): [7] Ouchemoukh S, Schweitzer P, Bachir BM, et al. HPLC sugar profiles of Algerian honeys[j]. Food Chem, 2010, 121(2): [8],,,. -,, [J]., 2006, 27(3): Mo HT, Li YK, Pan FY, et al. Determination of glucos,surcose,maltose and lactose in Low-surcose Foods by HPLC with an evaporative light-scattering detector[j]. Sci Technol Food Ind, 2006, 27(3): [9],,,. [J]., 2008, 29(6): Wu LM, Xue XF, Zhou X, et al. Determination of sugars in bee pollen by HPLC[J]. Food Sci, 2008, 29 (6): [10],. [J]. :, 2002, 32(4): Meng XL, Chen GH. TLC analysis oligochitosan[j]. J Ocean Univ Qingdao: Nat Sci, 2002, 32(4): [11],. [J]., 2001, 29(2): Wu H, Yang SH. High performance thin layer chromatography analysis of galactooligosaccharide and other sugars in the syrup[j]. China Dairy Ind, 2001, 29 (2): [12] Campa C, Baiutti E, Flamigni A. Capillary electrophoresis of sugar acids[j]. Methods Molecular Bio, 2008, 384(1): [13],,,., [J]., 2012, 33(8): Xiong JF, Zhou GM, Xu L, et al. Determination of glucose, sucrose and lactose in milk powder by ion chromatography[j]. Food Sci, 2012, 33 (8): [14] Qian WL, Khan Z, Watson DG, et al. Analysis of sugars in bee pollen and propolis by ligand exchange chromatography in combination with pulsed amperometric detection and mass spectrometry[j]. J Food Composition Anal, 2008, 21(1): [15],. [M]. :, Mou SF, Liu KN. Ion chromatography method and application [M]. Beijing: Chemical Industry Press, [16],. [M]. :, Ding MY, Tian SB. Ion Chromatography Principles and Applications [M]. Beijing: Tsinghua University Press, 作者简介 ( 责任编辑 : 邓伟 ) 蔡明明, 助理工程师, 主要研究方向为食品检验技术 [email protected] 任一平, 教授级高级工程师, 主要研究方向为卫生理化检验技术及食品安全检验技术 [email protected]

Microsoft Word 李爽.doc

Microsoft Word 李爽.doc 5 7 Vol. 5 No. 7 2014 7 Journal of Food Safety and Quality Jul., 2014 李爽 1, 陈启 1, 蔡明明 1, 任一平 2* (1., 310057; 2., 310051) 摘要 : 目的方法, C 18+ AQC, 结果, 4.65% 结论, 关键词 : ; ; ; Comparative study on quantification