5 5 Vol. 5 No. 5 2014 5 Journal of Food Safety and Quality May., 2014 - 竺 巧 玲 *, 俞 薇 ((), 315100) 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 315100, 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 :,, E-mail: 23743801@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 315100. E-mail: 23743801@qq.com
1520 5 - GB/T 20977-2007 [1] A, (),,,,,,, -,,,,,, [2-13],, -,,, 2 材 料 与 方 法 2.1 材 料 与 仪 器 ( Perkin Elmer ); (); (); ( G116305 ); ( ); ( ); A,, 0.1 mg/ml,, : 0.1 mg/ml 0 0.2 0.4 0.6 0.8 1.0 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, 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 0.1 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 +0.0001, r 2
5, : - 1521 0.9999, (0.02~0.1 mg/ml) (IU-PAC), 11, SD, 3SD/b 0.000647 mg/ml,, 0.032% (RSD), 3 表 2 稳 定 性 实 验 结 果 Table 2 Results of stability experiment (min) A 20 0.245 40 0.245 60 0.246 80 0.247 100 0.245 120 0.245 140 0.246 160 0.245 Fig. 2 2 Standard curve for determination of the content of total sugar 180 0.246 RSD 0.300 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 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 1.72 A 1, A 1.72, - 3.4 稳 定 性 实 验 A 0.2 ml, 2.2.2 620 nm 20 min 1, 2 h, 2 h, RSD 0.30%,, 2 3.5 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,, 4 98.5%, 96.2%, 97.0%, RSD 1.57%, 1.04%, 1.19%, - 3.7 与 国 家 标 准 方 法 ( 直 接 滴 定 法 ) 测 定 结 果 比 较 -, - 6, GB/T 20977-2007 [1] A ( ), 5,, 0.999,,,
1522 5 Table 4 表 4 加 标 回 收 率 实 验 结 果 Results of recovery test and calibration (mg) (mg) (mg) RSD 0.0299 0.020 0.0500 100.2 0.0299 0.020 0.0489 98.0 98.5 1.57 0.0299 0.020 0.0485 97.2 0.0299 0.030 0.0577 96.3 0.0299 0.030 0.0570 95.2 96.2 1.04 0.0299 0.030 0.0582 97.2 0.0299 0.040 0.0686 98.2 0.0299 0.040 0.0678 97.0 97.0 1.19 0.0299 0.040 0.0670 95.9 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 32.00, 4 结 论 --,,,,, 620 nm, C=0.2441A 620nm +0.0001, r 2 0.9999, 0.032%, RSD 1.72, RSD 2.07%, 98.5%, 96.2%, 97.0%,,, 参 考 文 献 [1]. GB/T 20977-2007 [S]. Chinese National Standardization Management Committee. GB/T 20977-2007General technical requirement for the pastry[s]. [2] ],,,. - [J]., 2008, 29(9): 499 502. 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): 499 502. [3],,. [J]., 2013, 7: 799 801. 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: 799 801. [4],. - [J]., 2005, 26 (7): 185 188. Wang LM, Xia WS. Determination of TPS by improvement of anthrone-sulfuric acidmethod[j]. Food Sci, 2005, 26 (7): 185 188. [5],. -[J]., 2011, 32(3): 399 401. Wei Y, Zhang SG. Determination of content of Lycium barbarum polysaccharide by anthrone-sulfuric acid method[j].sci Technol Food Ind, 2011, 32(3): 399 401. [6],,. - [J]., 2009, 30(8): 218 220. Li YL, Shi RJ, Zhang XZ. Determination of trehalose content of grifola frondosa mycelia by anthrone-sulfuric acid method[j].
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