Microsoft Word 孙稚菁-二校 出3371

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1 7 8 Vol. 7 No Journal of Food Safety and Quality Aug., 孙稚菁, 任国杰 *, 王灵芝, 李颖, 吴海霞, 李崇 (, ) 摘要 : 目的 ( ) ( ) 9 ( ) 方法,, 10 mmol/l -10 mmol/l ZORBAX SB-Aq(3.0 mm 150 mm, 3.5 μm), nm 结果, 0.1~100 mg/l, ~1.5 mg/kg 3, 90%~110%, (RSD) 10% 结论, 13 关键词 : ; ; Simultaneous determination of 13 kinds of food additives in sodas by high performance liquid chromatography SUN Zhi-Jing, REN Guo-Jie *, WANG Ling-Zhi, LI Ying, WU Hai-Xia, LI Chong (Dalian Institute Research Institute of Product Quality, Dalian , China) ABSTRACT: Objective To establish a method for the simultaneous determination of preservatives (benzoic acid and sorbic acid), sweet agents (acesulfame and saccharin sodium dehydrate) and colorants (hydrazine yellow, new red, naphthol red, acid blue 74, carmine, sunset yellow, allura red, brilliant blue and acid red 51) in sodas by high performance liquid chromatographic (HPLC). Methods Sodas samples were diluted to the right concentration by 10 mmol/l ammonium acetate. After filtered, the extract was separated on an ZORBAX SB-Aq column (3.0 mm 150 mm, 3.5 μm) using a gradient elution program with mobile phase of 10 mmol/l ammonium acetate - 10 mmol/l ammonium acetate methanol solution. Detection wavelengths were set at 230, 427, 507 and 620 nm, respectively. The qualitative analysis was based on chromatographic retention time and UV spectrum, and the quantitative analysis was performed by the standard curve method of peak area. Results The linear ranges of 13 analytes were in the range of 0.1~100 mg/l, with correlation coefficients more than The limits of quantiation (LOQs) were in the range of 0.5~1.5 mg/kg. The average recoveries at three spiked levels ranged from 90%~110% with RSDs less than 10%. * 通讯作者 :,,, fgrhrfy@163.com *Corresponding author: REN Guo-Jie, Master, Engineer, Dalian Institute Research Institute of Product Quality, Dalian , China. fgrhrfy@163.com

2 Conclusion This method is accurate, simple, sensitive and reliable, and can be used for the simultaneous determination of 13 kinds of food additives in sodas. KEY WORDS: sodas; food additives; high performance liquid chromatography 1 引言, 9,, ( ), 13 GB ,,,, [1],,,, [2] ( ) [3,4], ( ) [5],,, [6],, L-929, [7] 13,, 13 [1,8-12], - [13,14] [15] - [16] [17],,, 3, 8 [18] 13,,, 13, 13, ( ),, 2 实验部分 2.1 仪器与试剂材料 - (Agilent 1260, Agilent ); ( 0.1 mg 0.01 mg); ((XW-80A, ); (KQ-250DB, ); Dr. Ehrensorfer, 99%;, 98%; TCI, 98%; (, Merck ); (, Alfa Aesar ) 2.2 溶液配制 10 mmol/l : 0.77 g, 1000 ml,,,, 0.45 μm, 10 mmol/l 10 mmol/l : 0.77 g, 1000 ml,,,, 0.45 μm, 10 mmol/l : 10 mg( 0.1 mg), 10 ml,,, 1.0 mg/ml Ⅰ 10 mg( 0.1 mg), 10 ml,,, 1.0 mg/ml Ⅱ : 0.1 ml, 10 ml,, 100 μg/ml, μg/ml

3 8, : , 2.3 液相色谱分析参考条件 : Agilent poroshell 120 EC-C 18 (3.0 mm 100 mm, 2.7 μm) : A : 10 mmol/l ; B: 10 mmol/l : 0 2 min, 5%B 12%B; 2 7 min, 12%B; 7 12 min, 12%B 45%B; min, 45%B 80%B; min, 80%B 5%B; min, 5%B : nm : 35 : 0.5 ml/min : 2 μl 2.4 试样制备 5 min, 5.0 g( 1 mg) 25 ml, 10 mmol/l 25 ml,, 0.45 μm 3 结果与讨论 3.1 样品前处理条件的优化,,,,,, 10 mmol/l 5, 3.2 液相色谱条件优化 色谱柱的选择 C 18, C C 18, C 18,, 13, Aiglent poroshell 120 EC-C18 ZORBAX SB-Aq, ZORBAX SB-Aq, Aiglent ZORBAX SB-Aq 流动相的选择 A ( ), B ( ), 13,, B,,,,, 230 nm 5 min,,,,,, 10 mmol/l A, 10 mmol/l B,,, 紫外检测波长的优化 nm, 13, nm nm,, nm 427 nm,,, 427 nm 507 nm,,, nm 620 nm,, nm,,,, 13, 18 min ( 1) 3.3 线性范围与相关系数, 2.3,,, : μg/ml, 回收率与定量限 定量限,,, (S/N) S/N=3, S/N=10,

4 回收率 mg/kg 3, 6, 2, 91.8%~109.9%, (RSD) 10% 3.5 实际样品测定 70,,,,,, Fig. 1 Chromatograms of 13 kinds of food additives 1: (benzoic acid); 2: (acesulfame); 3: (sorbic acid); 4: (saccharin sodium dehydrate); 5: (hydrazine yellow); 6: (new red); 7: (naphthol red); 8: (acid blue 74); 9: (carmine); 10: (sunset yellow); 11: (allura red); 12: (brilliant blue); 13: (acid red 51)

5 8, : Table 1 表 1 13 种食品添加剂的线性回归方程 相关系数 检出限和定量下限 Regression equations, correlation coefficients, LODs and LOQs of 13 kinds of food additives (r 2 ) LOD/ (mg/kg) LOQ/ (mg/kg) 1 Y=8.102X Y=11.47 X Y=20.42 X Y=10.09 X Y=12.20 X Y=13.72 X Y=9.499 X Y=4.021 X Y=10.53 X Y=11.26 X Y=10.89 X Y=32.00 X Y=3.384 X Table 2 表 2 13 种食品添加剂的方法回收率和 RSD (n=6) Average recoveries and RSDs of 13 kinds of food additives (n=6) 100 mg/kg 10 mg/kg 1 mg/kg (%) RSD(%) (%) RSD(%) (%) RSD(%)

6 Fig. 2 Chromatograms of samples 4 结论 13,, 13,, 参考文献 [1],,,. 18 [J]., 2011, 21(2): Xiao HL, Tu HY, Wang HQ, et al. Rapid method for simultaneous determination of 18 water-soluble synthetic pigments in food by RP-HPLC [J]. Chin J Health Lab Technol, 2011, 21(2): [2],. [J]., 2006, 32(10): Mou GW, Li GH. The introduction of food preservatives and their determination technology [J]. Food Ferment Ind, 2006, 32(10): [3] Hannuksela M, Haahtela T. Hypersensitivity reactions to food additives [J]. Allergy, 1987, 42(8): [4] Safford RJ, Basketter DA, Allenby CF, et al. Immediate contact reactions to chemicals in the fragrance mix and a study of the quenching action of eugenol [J]. Br J Dermat, 1990, 123(5): [5] Howe GR, Burch JD, Miller AB, et al. Artificial sweeteners and human bladder cancer [J]. Lancet, 1977, 2(8038): [6],. [J]., 2006, 4: 27. Guo SP, Feng H. Production enterprises add oxathiazinone will bring what kind of harm to consumers in the Wine [J]. Superv Choice, 2006, 4: 27. [7],,. L-929 [J]., 2010, 24(1): Fu J, Wu CP, Zou ZF, Sodium benzoate and saccharin sodium, citric yellow joint toxicity to the cells of L 929 [J]. J Toxicol, 2010, 24(1): [8],,,. 7 [J]., 2015, 51(6): Zhang H, Gu Q, Yi XJ, et al. Determination of 7 synthetic colors and preservative in wine by HPLC transform wavelength [J]. Food Ferment Technol, 2015, 51(6): [9],,,. HPLC [J]., 2011, 21(5): Xiao L, Liu CM, Zhou JS, et al. Determination of acesulfame potassium, saccharin sodium and aspartame in drinks by HPLC [J]. Chin J Health Lab Technol, 2011, 21(5): [10],,,. HPLC [J]. ( ), 2007, 28(2): Wang LL, Song Y, Liu LL, et al. Quick test of contents of benzoic acid, saccharin acid and sorbicacidin soft drinks by using HPLC method [J]. J Bohai Univ (Nat Sci Ed), 2007, 28(2):

7 8, : [11],,. [J]., 2011, 27(5): 533, Chen DP, Yang FC, Zhang BY. Rapid determination of acesulfame, benzoicacid, sorbicacid and sodium saccharin in beverage by ultra performance liquid chromatography [J]. Mod Food Sci. Technol, 2011, 27(5): 533, [12],,. (UPLC) 6 [J]., 2010, 5: Gu H, Chen P, Liu WX. Simultaneous determining 6 kinds of coloring agent in beverage by UPLC [J]. Sci Technol. Innov Her, 2010, 5: [13],,,. - 7 [J]., 2015, 21(4): Liu D, Yang YY, Wang H, et al. Determination of 7 artificial sweeteners in drink using ultra performance liquid chromatography-tandem mass spectrometry [J]. Anal Test Technol Instrum, 2015, 21(4): [14],,,. - [J]., 2011, 29(11): Yin XH, Deng XJ, Yang H, et al. Determination of commonly abused dyes in food by liquid chromatography-tandem mass spectrometry [J]. Chin J Chromatogr, 2011, 29(11): [15],. 11 [J]., 2011, 21(4): Hou RX, Wu Q. Simultaneous determination of 11 Preservatives in foods by gas chromatography [J]. Chin J Health Lab Technol, 2011, 21(4): [16],,,. / / 7 [J]., 2010, 38(8): Chen Q, Ling Y, Zhang F, et al. Simultaneous determination of seven preservatives in beverage and jam using stir bar sorptive extraction and gas chromatography-tandem mass spetrometry [J]. Chin J Anal Chem, 2010, 38(8): [17],,,. [J]. -, 2015, 51(12): Chen ZT, Zhang R, Zheng XP, et al. Determination of sorbic acid and benzoic acid in wine by ion chromatography [J]. PTCA (Part B: Chem Anal), 2015, 51(12): [18],,. [J]., 2007, 36(2): Lv XL, Xu H, Lei YJ. The Determined simultaneously of many colorants, preservatives and sweeteners by high performance liquid chromatography [J]. Contem Chem Ind, 2007, 36(2): 作者简介 ( 责任编辑 : 白洪健 ) 孙稚菁, 高级工程师, 主要研究方向为食品和化工产品质量安全监测 @qq.com 任国杰, 硕士, 工程师, 主要研究方向为食品 药品 以及化妆品中功效成分及禁限用成分检测方法的研究与开发 fgrhrfy@163.com