Microsoft Word 胡玉霞-二校

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1 7 2 Vol. 7 No Journal of Food Safety and Quality Feb., 2016 胡玉霞 1, 汪立明 1, 王静 1, 徐琴瑶 1, 章柳柱 1, 郝云彬 (1., ; 2., ) 2* 摘要 : 目的方法 10%+0.1%,,, (0.2 μm), (SDS) -(74:26, V:V),, 结果 0.20~30 mg/l,, 0.999, 99.07%~110.33%, RSD 5% 结论,,,, 关键词 : ; ; ; ; Determination of nicotinic acid and nicotinamide in infant formula milk powder and rice powder by high performance liquid chromatography HU Yu-Xia 1, WANG Li-Ming 1, WANG Jing 1, XU Qin-Yao 1, ZHANG Liu-Zhu 1, HAO Yun-Bin 2* (1. Lin an Products Quality Inspection Center, Lin an , China; 2. School of Food Science and Technology, Jiangnan University, Wuxi , China) ABSTRACT: Objective To establish a method for the detection of nicotinic acid and nicotinamide in infant formula rice powder and milk powder by high performance liquid chromatography (HPLC). Methods Nicotinic acid and nicotinamide in infant formula powder and milk powder were extracted by 10% methanol and 0.1% phosphoric acid solution. After ultrasonic extraction, the samples were centrifuged to remove impurity. Then the extraction was filtered by syringe filter (0.2 μm), measured by HPLC with sodium dodecyl sulfate (SDS) buffer acetonitrile (74:26, V:V) as mobile phase and external standard method was used for quantification. Results The method showed a good linearity ranged from 0.20 to 30 mg/l of nicotinic acid and nicotinamide concentration with correlation coefficients above The recovery was 99.07%~110.33% and RSD was less than 5%. Conclusion Compared with the current standard method, this method is simple, and has low matrix interference, high accuracy, reproducibility, and high extraction efficiency, which is suitable for the rapid and batch determination of nicotinic acid and nicotinamide in infant formula rice powder and milk powder. KEY WORDS: nicotinic acid; nicotinamide; high performance liquid chromatography; rice powder; milk powder * 通讯作者 :,, yunbinhao@163.com *Corresponding author: HAO Yun-Bin, Senior Engineer, School of Food Science and Technology, Jiangnan University, Wuxi , China. yunbinhao@163.com

2 引言 B 3,, [1-3],, Ⅰ Ⅱ, Ⅰ Ⅱ,,,,,, [4-9],, [10-12] GB ( ) 70~360 g/100 kj, GB ( ) 110 g/100 kj [13,14],, [15],,, [16] [17] [18] [19-21] [22, 23] [24,25], [26], GB , 2 ph,,,,, [27],,,,,, 2 材料与方法 2.1 仪器与试剂 LC-20AD ( LC-20AD, SIL-20A, CTO-20A, SPD-M20A, ); DS-5510DTH (40 KHZ, ); DK-S24 ( ); Milli-Q ( Millipore ); Sartorius PB-10 (() ) (, ); (, ); (); (): () 2.2 实验方法样品前处理 1.5~2 g( g) 50 ml, 2 g/100 ml 5.0 ml, 60 1 h (10%+0.1% )25 ml, 10 min,,, r/min 5 min, 0.22 μm, HPLC 色谱条件 GL Wondasil TM C 18 (250mm 4.6 mm, 5 μm), 35, : (74:26, V:V), 1.0 ml/min,: 261 nm, : 20 μl 3 结果与讨论 3.1 样品称样量的影响, 2.2.1, 50 ml, 3 g,, 2, 20%,

3 2, : 841, -NH 2, ; 1.5~2 g,, 2%, 3.2 提取试剂的影响,,, 10% 0.1%, 2.2.1, GB ,,,,, 0~60%,,, 85%,, 10%, 40%,,, 3.3 磷酸比例的影响, 0~1%,, 10% 90%, 0.1%, 3.4 方法学评价,, 3,,, 6,, 1 2~4 Fig. 1 1 (n=3) Comparison of different solvents on extraction rate of milk powder and rice powder (n=3)

4 842 7 表 1 烟酸和烟酰胺的线性范围, 线性方程, 相关系数, 回收率, 定量限 (n=6) Table 1 The linear range, linear equation, correlation coefficient, recovery rate, and limit of quantitation of nicotinic acid and nicotinamide. (n=6) (mg/l) r 2 ( mg/kg) 0.20~30 Y= X (mg/100 g) ( mg/100 g) /% RSD/% ND (mg/l) r 2 (mg/kg) 0.20~30 Y= X (mg/100 g) (mg/100 g) /% RSD/% : ND Fig.2 2 Chromatogram of standard samples 3.5 实际样品的检测 6 6, 2, 1.3%~60.6%;, 0%~53.6%, 25.8%~62.7%;, -14.3%~30.7% [10,11],,,,

5 2, : 843 Fig. 3 3 Chromatogram of milk powder samples Fig. 4 4 Chromatogram of rice flour samples 表 2 实际样品检测结果 (n=6) Table 2 Detection results of real samples (n=6) mg/100 g ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ±0.15

6 844 7 续表 2 mg/100 g ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ±0.14 : 1~6, 4 6, 2, 4 结论,,,,, GB ,, 0.20~30 mg/l,, , %~110.33%, RSD 5%,, 参考文献 [1],,. [M]. :, Jiang PZ, Cai MQ, Guo HW. Nutritional imbalance and health [M]. Beijing: Chemical Industry Press, [2] Grundy SM, Mok HY, Zech L, et al. Influence of nicotinic acid on metabolism of cholesterol and triglycerides in man[j]. J Lipid Res, 1981, 22(1): [3] Moreschi ECP, Matos JR, Almeida-Muradian LB. Thermal analysis of vitamin PP Niacin and Niacinamide [J]. J Therm Anal Calorim, 2009, 98(1): [4] Katrina L, Bogan, Charles B. Nicotinic acid, nicotinamide, and nicotinamide riboside: a molecular evaluation of NAD + precursor vitamins in human nutrition [J]. Annu Rev Nutr, 2008, 28: [5],. 50 [M].,. :, Mcgowan M, Mcgowan J. The 50 methods of lowering cholesterol [M]. Lei LP, trans. Beijing: Xinhua Press, [6] Ohashi R, Mu H, Wang X, et a1. Reverse cholesterol transport and cholesterol efflux in atherosclerosis [J]. J Assoc Physic, 2005, 98(12): [7] Ahsehul R, Hoffer A, Stephen JD. Influence of nicotinic acid on serum cholesterol in man [J]. Archives Biochem, 1955, 54(2): [8] Carlson LA. Nicotinic acid: the broad-spectrum lipid drug. A50th anniversary review [J]. J Int Med, 2005, 25(8): [9] Revollo JR, Grimm AA, Imai S. The regulation of nicotinamide adenine dinucleotide biosynthesis by Nampt/PBEW/visfatin in mammals [J]. Curt Opin Gastroenterol, 2007, 23(2): [10]. [M]. :, Gao YC. Nutrition [M]. Beijing: Beijing Sport University Press, [11] Luo QF, Sun L, Du GH, et al. Progress in new drugs targeting reverse cholestero transport [J]. J Chin Pharmacol Bull, 2006, 122(8): [12] Kenneth M, Zhao ZC. Nicotinamide: necessary nutrient emerges as anovel cytoprotectant for the brain [J]. Trends Pharmacol Sci, 2003, 24(5): [13] GB [S] GB National food safety standard infant formula [S]. [14] GB [S] GB National food safety standard older infants and young children formula [S]. [15],,,. [J]., 2011, 32(16): Huo YM, Wang YL, Wang J, et al. Uncertainty evaluation for nicotinamide determination in infant formula milk powder by high performance liquid chromatography [J]. Food Sci, 2011, 32(16): [16]. B 2, B 3 [J].

7 2, : 845, 2003, 21(6): Guo YD. Simultaneous determination of riboflavin, nicotinic acid and nicotinamide by supercritical fluid chromatography [J]. Chin J Chromatogr, 2003, 21(6): [17] Saccania G, Tanzia E, Mallozzia E, et al. Determination of niacin in fresh and dry cured pork products by ion chromatography: experimental design approach for the optimisation of nicotinic acid separation [J]. Food Chem, 2005, 92(2): [18] Manuela P, Emilia M, Silvia R, et al. Liquid chromatography/electrospray ionization tandem mass spectrometry assay for determination of nicotine and metabolites, caffeine and arecoline in breast milk [J]. Rapid Commun Mass Spectr, 2007, 21(16): [19] Tania S, Agostini1 HT. Simultaneous determination of nicotinamide, nicotinic acid, riboflavin, thiamin, and pyridoxine in enriched Brazilian foods by HPLC [J]. J High Res Chromatogr, 1997, 20(4): [20] Lahély S, Bergaentzlé M, Hasselmann C. Fluorimetric determination of niacin in foods by high-performance liquid chromatography with post-column derivatization [J]. Food Chem, 1999, 65(1): [21],,,. B 6 [J]., 2015, 33(3): Fan JP, Xu ZD, Chen J, et al. HPLC determination of niacin, nicotinamide and itamin B6 in milk power [J]. Pack Food Mach, 2015, 33(3): [22] Roman L, Erkan FY, Rudolf E, et al. Quantitative Investigation of trigonelline, nicotinic acid, and nicotinamide in foods, urine, and plasma by means of LC-MS/MS and stable isotope dilution analysis [J]. Food Chem, 2008, 56 (23): [23] Daniel P, Carmen MD, Adriana F. Fast simultaneous analysis of caffeine, trigonelline, nicotinic acid and sucrose in coffee by liquid chromatography mass spectrometry [J]. Food Chem, 2008, 110(4): [24] Tadashi M, Isao K, Shuichi S. Rapid determination of nicotinic acid by immobilized lactobacillus arabinosus, 1978, 99(2): [25] GB [S]. GB National food safety standard determination of vitamin niacin and niacinamide in foods for infants and young children, milk and milk products [S]. [26] Mu GF, Luan F, Liu HT, et al. Use of experimental design and artificial neural networkin optimization of capillary electrophoresis for the determination of nicotinic acid andnicotinamide in food compared with high-performance liquid chromatography [J]. Food Anal Methods. 2013, (6): 作者简介 ( 责任编辑 : 金延秋 ) 胡玉霞, 工程师, 主要研究方向为食品安全与营养 hyxzxf@163.com 郝云彬, 高级工程师, 主要研究方向为水产品质量安全 yunbinhao@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