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1 5 5 Vol. 5 No Journal of Food Safety and Quality May., 竺巧玲 *, 俞薇 ((), ) 摘要 : 目的 -, 方法 -,, 结果 620 nm, 0.032%, RSD 1.72, RSD 2.07%, 98.5%, 96.2%, 97.0%,,,, 结论,, 关键词 : ; ; - Determination of content of total sugar in cake by anthrone-sulfuric acid method ZHU Qiao-Ling *, YU Wei (Ningbo Yinzhou Measurement and Test Center for Quality and Technique Supervising (Food Safety Testing Center of Yinzhou District), Ningbo , China) ABSTRACT: Objective To establish a new method for determination of total sugar in cake by using the anthrone sulphuric acid for the first time. Methods Wavelength, precision, stability, repeatability and recovery rate were measured respectively by the anthrone-sulfuric acid method, and with the national standard of the measured results were compared to evaluate. Results The detection wavelength was 620 nm, the detection limit of the method was 0.032%, the RSD of precision experiment was 1.72%, the RSD of repeatability experiment was 2.07%, the average recovery rate was 98.5%, 96.2%, 97.0% respectively. This method had a good stability. Compared with the national standard method, these two measurement results were basically the same without statistically significant difference. Conclusion The method is simple and rapid, with low detection limit, accuracy, high precision and repeatability, and have a higher practical application value, which can replace the direct titration method to satisfy the analysis for cake total sugar daily inspection requirements. KEY WORDS: cake; total sugar; anthrone sulfuric acid method 1 引言,,,,,,, * 通讯作者 :,, @qq.com *Corresponding author: ZHU Qiao-Ling, Quality Engineer, NingboYinzhou Measurement and Test Center for Quality and Technique Supervising(Food Safety Testing Center of Yinzhou District), No. 258, Huifeng East Road,Yinzhou District, Ningbo @qq.com

Technique Supervising (Food Safety Testing Center of Yinzhou District), Ningbo 315100, China) ABSTRACT: Objective To establish a new method for determination of total sugar in cake by using the

2 GB/T [1] A, (),,,,,,, -,,,,,, [2-13],, -,,, 2 材料与方法 2.1 材料与仪器 ( Perkin Elmer ); (); (); ( G ); ( ); ( ); A,, 0.1 mg/ml,, : 0.1 mg/ml ml, 1.0 ml, 72% 0.05% 5 ml,, 15 min, 20 min 1 cm, : 0.2 ml, 1.0 ml, 0.05% 5 ml,, 15 min, 20 min, X=C V 100/(m D 1000), X ; C= (mg); V=(mL); m= (g); D=(mL) 3 结果与分析 3.1 最佳测定波长的确定 0.5 ml A 0.2 ml,, 500~720 nm, 检测方法 [1] 蛋糕总糖提取工艺流程 0.25 g( g), 100 ml, 50 ml ( GB/T [14], ) 30 min( ), 5 ml 5 ml,, ( 1:1 )10 ml, min, 1, 20%, 250 ml,,, [15] 蛋糕总糖含量的测定 - 蒽酮 - 硫酸比色法 : g,, 1000 ml, 1 Fig. 1 The determination of optimum wavelength 1, 620 nm, 620 nm 3.2 标准曲线回归方程与方法检出限 620 nm,,, ( 2), C=0.2441A 620nm , r 2

2 ml,, 500~720 nm, 1 2.2 检测方法 [1] 2.2.1 蛋糕总糖提取工艺流程 0.25 g( 0.0001 g), 100 ml, 50 ml ( GB/T 6682-2008 [14], ) 30 min( ), 5 ml 5 ml,, ( 1:1 )10 ml, 70 10 min, 1, 20%, 250 ml,,, [15] 2.2.2 蛋糕总糖含量的测定 - 蒽酮 - 硫酸比色法 : 105 0.

3 5, : , (0.02~0.1 mg/ml) (IU-PAC), 11, SD, 3SD/b mg/ml,, 0.032% (RSD), 3 表 2 稳定性实验结果 Table 2 Results of stability experiment (min) A Fig. 2 2 Standard curve for determination of the content of total sugar RSD 表 3 重现性实验结果 Table 3 Results of repeatability experiment 3.3 精密度实验 A 6, (RSD), 1 A RSD Table 1 表 1 精密度实验结果 Results of precision experiment RSD A 1, A 1.72, 稳定性实验 A 0.2 ml, nm 20 min 1, 2 h, 2 h, RSD 0.30%,, 重现性实验, A 6, 2.2.1, 3, 6 A 2.07, 3.6 加标回收率实验 A 0.1 ml 3,,, 3,, %, 96.2%, 97.0%, RSD 1.57%, 1.04%, 1.19%, 与国家标准方法 ( 直接滴定法 ) 测定结果比较 -, - 6, GB/T [1] A ( ), 5,, 0.999,,,

3 精密度实验 A 6, (RSD), 1 A RSD 29.15 29.35 30.55 29.55 30.45 30.35 29.90 0.619 2.07 Table 1 表 1 精密度实验结果 Results of precision experiment RSD 29.95 29.35 30.55 29.35 30.20 30.05 29.88 0.515 1.

4 Table 4 表 4 加标回收率实验结果 Results of recovery test and calibration (mg) (mg) (mg) RSD Table 5 表 5 两种方法的测定结果比较 Comparison of the determination results of two methods - A B C D E F , 4 结论 --,,,,, 620 nm, C=0.2441A 620nm , r , 0.032%, RSD 1.72, RSD 2.07%, 98.5%, 96.2%, 97.0%,,, 参考文献 [1]. GB/T [S]. Chinese National Standardization Management Committee. GB/T General technical requirement for the pastry[s]. [2] ],,,. - [J]., 2008, 29(9): Liang LJ, Zeng ZL, Xiong T, et al. Determination of content of polysaccharide in garlic seed by anthrone-sulfuric method[j]. Food Sci, 2008, 29(9): [3],,. [J]., 2013, 7: Fan CY, Tao ZM, Wu ZG. Comparison of phenol sulfuric acid method and anthrone sulfuric acid method for the determination of content of polysaccharides in Dendrobium candidum[j]. Zhejiang Agric Sci, 2013, 7: [4],. - [J]., 2005, 26 (7): Wang LM, Xia WS. Determination of TPS by improvement of anthrone-sulfuric acidmethod[j]. Food Sci, 2005, 26 (7): [5],. -[J]., 2011, 32(3): Wei Y, Zhang SG. Determination of content of Lycium barbarum polysaccharide by anthrone-sulfuric acid method[j].sci Technol Food Ind, 2011, 32(3): [6],,. - [J]., 2009, 30(8): Li YL, Shi RJ, Zhang XZ. Determination of trehalose content of grifola frondosa mycelia by anthrone-sulfuric acid method[j].

9 Table 5 表 5 两种方法的测定结果比较 Comparison of the determination results of two methods - A 29.88 29.60 B 20.30 20.55 C 18.65 18.50 D 19.50 19.69 E 25.36 25.56 F 32.16 32.

5 5, : Food Sci, 2009, 30(8): [7],,,. - 3,5- [J]., 2010, 31(10): Li Q, Tang W, Shi YY, et al. Determination of polysaccharide in water extraction from eucommia ulmoides oliver by 3,5-dinitrosalicylic acid(dns)method and anthrone-sulfuric method[j]. Sci Technol Food Ind, 2010, 31(10): [8],,. [J]., 2013, (17): Weng X, Xin G, Li YX. Study on determination conditions of total sugar from potato starch by anthrone colorimetry[j]. Food Res Development, 2013, (17): [9],,,. [J]., 2009, 34(9): Liu XH, Cheng YG, Lin L, et al. Comparison of methods in determination of polysaccharide in Lycium barbarum L[J]. Food Sci Technol, 2009, 34(9): [10],,. - [J]., 2012, 33(24): Zhang H, Wang T, Li CQ. Determination of polysaccharides from mulberry leaf by optimization of anthrone-sulfuric acid method by response surface methodology[j]. Sci Technol Food Ind, 2012, 33(24): [11],,,. [J]., 2005, 21(3): Wen CF, Dong AW, Li GZ, et al. Determination of total sugar and reducing sugar in viola philippicassp munda W. becker by anthrone colorimetry[j]. Guangzhou Food Sci Technol, 2005, 21(3): [12],. [J]., 2013, 13(4): Li XX, Li JZ. Determination of the content of soluble sugar in sweet corn with optimized anthrone colorimetric method[j]. Storage Process, 2013, 13(4): [13],,,.- [J]., 2006, 22(1): Tan HG, Mei YJ, Guan FM, et al. Determination of trehalose content by anthrone-sulphuric acid colorimetric method [J]. Guangzhou Food Sci Technol, 2006, 22(1): [14]. GB/T [S]. Chinese National Standardization Management Committee. GB/T Water for analytical laboratory use-specification and test methods[s]. [15]. [M]. :, Dalian Institute of Light Industry.Food analysis[m]. Beijing: Chinese Light Industry Press, 作者简介 ( 责任编辑 : 邓伟 ) 竺巧玲, 质量工程师, 主要研究方向为食品质量管理和食品安全检测 @qq.com

[8],,. [J]., 2013, (17): 86-88. Weng X, Xin G, Li YX. Study on determination conditions of total sugar from potato starch by anthrone colorimetry[j]. Food Res Development, 2013, (17): 86 88. [9],,,.

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