Microsoft Word 出1870

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1 8 5 Vol. 8 No Journal of Food Safety and Quality May., 2017 B 1 B 2 B 6 陈彩云 *, 魏鲜娥, 蔡伟江, 黎小兰, 张喜金 (, ) 摘要 : 目的 B 1 B 2 B 6 方法 0.2%, Alltima-C 18, -5 mmol/l, (diode array detector, DAD) 200 nm 280 nm 结果 B 1 B 2 B 6,, 93.9%~103.2%, (relative standard deviation, RSD) 0.4%~1.8% 结论, B 1 B 2 B 6 关键词 : ; ; B 1 ; B 2 ; B 6 ; Determination of pantothenate, nicotinamide, vitamin B 1, vitamin B 2, and vitamin B 6 in healthy food by high performance liquid chromatography CHEN Cai-Yun *, WEI Xian-E, CAI Wei-Jiang, LI Xiao-Lan, ZHANG Xi-Jin (By-Health Co., Ltd., Zhuhai , China) ABSTRACT: Objective To establish a method for the simultaneous determination of pantothenate, nicotinamide, vitamin B 1, vitamin B 2 and vitamin B 6 in healthy food by high performance liquid chromatography (HPLC). Methods Samples were ultrasonically extracted with 0.2% phosphoric acid solution, separated by alltima-c 18 column with acetonitrile-5 mmol/l sodium heptanesulfonate solution as the mobile phase for gradient elution, and then detected by diode array detector (DAD) simultaneous at the wavelengths of 200 nm and 280 nm. Results Pantothenate, nicotinamide, vitamin B 1, vitamin B 2 and vitamin B 6 could be completely separated, and they also had good linear relationships in their linear ranges. The average recoveries were 93.9%~103.2%. The relative standard deviations were 0.4%~1.8%. Conclusion This method is rapid, simple, accurate and repeatable, which can be used for the simultaneous determination of pantothenate, nicotinamide, vitamin B 1, vitamin B 2 and vitamin B 6 in healthy food. KEY WORDS: pantothenate; nicotinamide; vitamin B 1 ; vitamin B 2 ; vitamin B 6 ; high performance liquid chromatography * 通讯作者 :, @qq.com *Corresponding author: CHEN Cai-Yun, By-Health Co., Ltd., Zhuhai , China @qq.com

2 5, : B 1 B 2 B 引言,,,,,,, A B 2, B 1 C,,,, (high performance liquid chromatography, HPLC) [1-10], 1, B 6 B 2 B 1 5, 5,,,, 2 材料与方法 2.1 仪器与材料 Agilent 1260 (, (diode array detector, DAD)); XP 205 ( - ); KQ-500VDE ( ) B, D D D, (, ) (, ) (, ); ( : 99.9%, Supelco, : LC10011V); ( :99.9%, Supelco, :LC01839V); B 1 ( : 99.9%, Supelco, : LB84083V); B 2 ( : 98.7%, Dr.Ehrenstorfer GmbH, : D0144); B 6 ( : 99.9%, Supelco, : LB83988V) 2.2 试验方法色谱条件 : Alltima C 18 (4.6 mm 150 mm, 5 μm); : 1.0 ml/min; : 40 ; : 10 μl; : 200 nm 280 nm; : (diode array detector, DAD); : A 5 mmol/l, B, 1 表 1 梯度洗脱程序 Table 1 Gradient elution program (min) A (%) B (%) 标准溶液的制备 (1) 12 mg 35 mg 5 mg B 1 5 mg B 2 5 mg B 6 ( 0.01 mg), 100 ml, 1 ml, ( ),, 0.45 μm, 4 (2), 0.45 μm, 10 μl, c(mg/ml), A, 样品前处理 20,,, 1.0 g 50 ml, 0.2%, 40 ( 500 W, 50 khz) ( 25 min),, 0.2%,,, 0.45 μm, 3 结果与分析 3.1 溶剂的选择 5, B 1 B 6 4, B 2, B 2,,, B 2, 0.2%,,,, 0.2% 3.2 流动相的选择 5,,,, C 18,, -, -, -, -, - -,,

3 1868 8,,,,,, 5 1.5,,,, mol/l, 5,,,,,, B 1 B 2 B 6 5,, -,, ( 1) 3.3 波长的选择,,, 4 5, 200 [11] [12] 444 [13] B 1 B 2 B 6 ( 2),, 200 nm,, ; nm nm, B 1 B 2 B 6, 260 nm, B 6, 444 nm B 1 B nm, 5, 200 nm 280 nm B 1 B 2 B 方法学考察方法的线性,, B 1 B 2 B ~0.60 mg/ml, R , 检出限与定量限, 3 (limit of detection, LOD), 10 (limit of quantification, LOQ), ( 3) 精密度试验, 6,, B 6 B 2 B 1, (relative standard deviations, RSD) 0.1% 1 B 1 B 2 B 6 Fig. 1 Gradient elution chromatograms of calcium pantothenate, nicotinamide, vitamin B 1, vitamin B 2 and vitamin B 6

4 5, : B 1 B 2 B Fig. 2 2 B 1 B 2 B 6 Chromatograms of calcium pantothenate, nicotinamide, vitamin B 1, vitamin B 2 and vitamin B 6 at different wavelengths 表 2 泛酸钙烟酰胺维生素 B 1 维生素 B 2 和维生素 B 6 的线性关系 Table 2 Linear relationships of calcium pantothenate, nicotinamide, vitamin B 1, vitamin B 2 and vitamin B 6 R (mg/ml) Y=11941X ~ Y=1715X ~ B 6 Y=16716X ~ B 2 Y=29822X ~ B 1 Y= 7896X ~

5 表 3 泛酸钙烟酰胺维生素 B 1 维生素 B 2 和维生素 B 6 的检出限与定量限 (n=6) Table 3 Limits of detection and limits of quantification of calcium pantothenate, nicotinamide, vitamin B 1, vitamin B 2 and vitamin B 6 (n=6) (μg/ml) (μg/ml) B B B B 2 B 6 5, 表 5 加标回收率和相对标准偏差 (n=3) Table 5 The recoveries and RSDs (n=3) (mg) (%) RSD(%) 重复性试验 B, 6, B 6 B 2 B 1, RSD 4 表 4 泛酸钙烟酰胺维生素 B 1 维生素 B 2 和维生素 B 6 5 种成分的重复性 (n=6) Table4 Repeatabilities of calcium pantothenate, nicotinamide, vitamin B 1, vitamin B 2 and vitamin B 6 (n=6) (mg/100 g) RSD(%) ~ ~ B ~ B 6 B 2 B B ~ B ~ 方法回收率 9, 3, 3, 50 ml, 0.2%, mg; mg B mg B mg B mg,, %~103.2%, RSD 0.4%~1.8%, B 1 B 2 B 6 4 结论 HPLC, B 1 B 2 B 6,, B 1 参考文献 [1]. HPLC (15) B 1 B 2 B 6 [J]., 2012, 15(5): Wang WJ. Determination of nicotinamide, vitamin B 1, vitamin B 2 and vitamin B 6 in Duoweiyuansu capsules (15) by HPLC [J]. China Pharm, 2012, 15(5): 6 10 [2]. B1 B2 [J]., 2016, 16(8): Zeng YM. Content determination of vitamin B 1, vitamin B 2 in compound hepar extrectum tables by HPLC [J]. Eval Anal Drug-Use Hosp China, 2016, 16(8): [3]. HPLC 5 B [J]., 2016, (1): 21 23, 38. Liang L. Simultaneous determination of 5 kinds of vitamin B in vitamin premix feed by HPLC [J]. China feed, 2016, (1): 21 23, 38. [4]. HPLC B B 1 B 2 B 6 [J]., 2012, 26(8): Han XM. Determination of vitamin B 1, vitamin B 2 and vitamin B 6 in compound vitamin B tablets by HPLC [J]. Chin Pharm Aff, 2012, 26(8): [5]. HPLC B 1 B 2 [J]., 2015, 26(18):

5, : B 1 B 2 B 6 1871 Li DF. Content determination of vitamin B 1 and vitamin B 2 in trivitamin and calciun gluconate, calcium hydrogen phosphate chewable tablets by HPLC [J].

6 5, : B 1 B 2 B Li DF. Content determination of vitamin B 1 and vitamin B 2 in trivitamin and calciun gluconate, calcium hydrogen phosphate chewable tablets by HPLC [J]. China Pharm, 2015, 26(18): [6]. 3 [J]., 2012, 21(22): He X. Reversed-phase ion-pair chromatography method for the determination of three water soluble vitamins compound vitamin tables [J]. Chin J New Drugs, 2012, 21(22): [7]. 5 [J]., 2011, 17(1): Hua YY. Determination of 5 water-soluble vitamins in health food by high performance liquid chromatography [J]. Strait J Prev Med, 2011, 17(1): [8]. B 1 B 6 C [J]., 2012, 32(9): Jin PF. Simutaneous determination of vitamin B 1, vitamin B 6, vitamin C, niacinamide and pantothenic acid in vitamins with minerals tablets by HPLC [J]. China J Pharm Anal, 2012, 32(9): [9]. B [J]. -, 2010, 46(5): Xu H. Simultaneous determination of six B-group vitamins in functional drinks by HPLC [J]. Phys Test Chem Anal Part B, 2010, 46(5): [10]. [J]., 2011, (10): Zuo CY. The present situation and the international standard test methods of vitamin [J]. China Food Saf, 2011, (10): [11]. HPLC B 1 B 2 B 6 [J]., 2015, (29): Sun JJ. Determination of vitamin B 1, vitamin B 2 and vitamin B 6 in five vitamins lysine granules by HPLC [J]. Med Health Manag, 2015, (29): [12]. B B1 B2 [J]., 2016, 33(3): Guo QS. A Quantiative nmr method to analyze vitamin B 1, vitamin B 2, nicotinamide and calcium pantothenate contents in compound vitamin B tablets [J]. Chin J Magn Reson, 2016, 33(3): [13] GB [S] GB Determination of pantothenic acid in foods for infants and young children, milk and milk products[s]. [14] GB/T [S]. GB/T Determination of thiamine hydrochloride, pyridoxine hydrochioride, niacin, niacinamide and caffeine in health foods[s]. [15]. ( )[M]. :, Chinese Pharmacopoeia Commission. The People's Republic of China pharmacopoeia (part two) [M]. Beijing: Chinese Medical Science and Technology Press, 作者简介 ( 责任编辑 : 姜姗 ) 陈彩云, 主要研究方向为保健食品的质量检测 @qq.com

Microsoft Word 王德伟-二校 3088

Microsoft Word 王德伟-二校 3088 6 8 Vol. 6 No. 8 2015 8 Journal of Food Safety and Quality Aug., 2015 王德伟 *, 游景水, 黄远英 (, 519040) 摘要 : 目的 (RP-HPLC) 方法 (ph 4.6), RP-HPLC, ph4.6, C 18, A 0.1%, B 0.09%(V:V) 90%(V:V),, 214 nm, 0.7 ml/min