8 6 Vol. 8 No. 6 2017 6 Journal of Food Safety and Quality Jun., 2017-1, 2, 孔庆龙, 余汪平, 郭冬梅, 朱卓, 侯代松 3, 游燕 (1., 650111; 2., 650111; 3., 650111) 1, 2, 3* 摘要 : 目的 方法 -, - 490 nm 结果 -,, 0.02~0.1 mg/ml, r 2 =0.9998, 99.89% 结论 - 关键词 : ; ; -; Determination of polysaccharide in the alcoholic drink of SanqiGouqi by phenol-sulfuric acid colorimetry method KONG Qing-Long 1,2,3, YU Wang-Ping 1,2,3, GUO Dong-Mei 1,2,3, ZHU Zhuo 1,2,3, HOU Dai-Song 1,2,3, YOU Yan 1,2,3* (1. Yunnan Institute of Materia Medica, Kunming 650111, China; 2. Yunnan Bai Yao Group Innovation and R&D Center, Kunming 650111, China; 3. Yunnan Province Company Key Laboratory for TCM and Ethnic Drug of New Drug Creation, Kunming 650111, China) ABSTRACT: Objective To establish a method for determination of polysaccharide content in the alcoholic drink of SanqiGouqi. Methods The phenol-sulfuric acid colorimetry method was performed at wavelength of 490 nm with phenol-sulfuric acid as a color reagent. Results The phenol-sulfuric acid colorimetry method had stability and high precision for determination of polysaccharide in the alcoholic drink of SanqiGouqi. The good positive linear relationship was shown in the range of 0.02~0.1 mg/ml, the correlation coefficient (r 2 ) was 0.9998, and the average recovery rate of added samples was 99.89%. Conclusion The established method is suitable for determination of polysaccharide in the alcoholic drink of SanqiGouqi. KEY WORDS: polysaccharide; alcoholic drink of SanqiGouqi; phenol-vitriolic colorimetry; content determination 1 引言,,, [1-5] [6,7] ; [8-10] [11] [12] [13], 2,,,, [14],,, * 通讯作者 :,, E-mail: yy81221@ynby-yimm.com *Corresponding author: YOU Yan, Senior Engineer, Yunnan Institute of Materia Medica, No.24, Lengshuitang, Bijie Town, Xishan District, Kunming 650111, China. E-mail: yy81221@ynby-yimm.com
2268 8 [15], -,,,, 2 材料与方法 2.1 材料与仪器 ( ); (, ); (, ) AG285 ( - ); ( ); UV2501 () 2.2 实验方法 2.2.1 葡萄糖标准溶液的制备 10.0 mg, 100 ml,, 0.1 mg/ml, 2.2.2 供试样品的制备 100 ml, 4,,,, 100 ml,, 100 ml 2.2.3 标准曲线的绘制 0.2 0.4 0.6 0.8 1.0 ml, 20 ml, 1 ml,, 5% 1 ml, 5 ml, 20 min, 490 nm A,, 2.2.4 样品分析 0.1 ml, 20 ml, 2.2.3, 1 ml,,,, Table 1 表 1 乙醇加入量对吸光值的影响 Effect of ethanol volume on the absorbance / 2 1.211 3 1.985 4 2.078 5 2.099 4 5,, 4 3.2 水浴时间 15 20 25 30 min, 2 Table 2 表 2 水浴时间对吸光值的影响 Effect of water bath time on the absorbance /min 15 0.189 20 0.205 25 0.209 30 0.208,,, 20 min 3.3 方法学考察 3.3.1 标准曲线的绘制 Y=10.182X-0.0146, r²=0.9998, 0.02~0.1 mg/ml, 1 3 结果与分析 3.1 乙醇加入量的选择 -,,,,, 2 3 4 5, 1 1 Fig. 1 Standard curve 3.3.2 精密度试验 0.6 ml,, 490 nm 6, RSD 0.43%,, 3
6, : - 2269 表 3 精密度试验 Table 3 Precision test 1 0.600 2 0.599 3 0.597 4 0.603 5 0.601 6 0.604 0.601 RSD/% 0.43 3.3.3 稳定性试验 1, 490 nm, 0 5 10 15 20 25 30 min, RSD 0.76%, 30 min, 4 表 4 稳定性试验 Table 4 Stability test 3.3.4 重复性试验 5, 490 nm, RSD 1.29%,, 5 表 5 重复性试验 Table 5 Repeatability test 1 0.203 2 0.199 3 0.206 4 0.201 5 0.203 0.202 RSD/% 1.29 /min 0 0.203 5 0.205 10 0.207 15 0.207 20 0.207 25 0.207 30 0.207 0.206 RSD/% 0.76 3.3.5 加样回收试验 0.2 ml 3 20 ml, 0.3 0.4 0.5 ml, 490 nm, 6 6, 98.86%~101.26%, 99.89%, 3.4 样品测定 5, 0.1 ml, 490 nm, 7, 100 ml 21.59 mg Table 6 表 6 加样回收试验 Recovery of added samples test /mg /mg /mg /% /% RSD/% 0.04 0.03 0.701 0.0703 100.94 0.04 0.03 0.699 0.0701 100.28 0.04 0.03 0.702 0.0704 101.26 0.04 0.04 0.798 0.0798 99.52 0.04 0.04 0.797 0.0797 99.27 0.04 0.04 0.795 0.0795 98.78 0.04 0.05 0.903 0.0901 100.24 0.04 0.05 0.896 0.0894 98.86 0.04 0.05 0.901 0.0899 99.85 100.83 0.50 99.19 0.38 99.65 0.71
2270 8 表 7 样品测定 Table 7 Determination of samples /(mg/ml) /mg (mg) 1 0.206 0.0217 21.67 2 0.206 0.0217 21.67 3 0.203 0.0214 21.4 21.59 4 0.208 0.0219 21.9 5 0.202 0.0213 21.3 4 结论 -,, 0.02~0.1 mg/ml, r 2 =0.9998, 99.89%-,, 4 5,, 4 15~30 min,,, 20 min,,,,, 参考文献 [1] Gao H, Wang F, Lien EJ, et al. Immunostimulating polysaccharides from Panax notoginseng [J]. Pharm Res, 1996, 13: 1196 1200. [2] Zhu Y, Pettolino F, Mau SL, et al. Characterization of cell wall polysaccharides from the medicinal plant Panax notoginseng [J]. Phytochemistry, 2005, 66: 1067 1076. [3] Zhu Y, Pettolino F, Mau SL, et al. Immunoactive polysaccharide-rich fractions from Panax notoginseng [J]. Planta Med, 2006, 72: 1193 1199. [4] Wu YL, Wang D. Structural characterization and DPPH radical scavenging activity of an arabinoglucogalactan from Panax notoginseng root [J]. J Nat Prod, 2008, 71: 241 245. [5],,,. [J]., 2016, 31(6): 573 576. Zhong YY, Yang XH, Zhang YW, et al. Impact of Panax polysaccharides on immune function in mice [J]. West China J Pharm Sci, 2016, 31(6): 573 576. [6],,,. [J]., 2009, 18(2): 184 185. Chen W, Zhang YC, Zhou MM, et al. Experimental study on effect of the polysaccharides in Panax notoginseng on oxidation index of the rat serum under the microwave radiation [J]. Chin Radiol Health, 2009, 18(2): 184 185. [7],,, [J]., 2015, 32(11): 996 998. Li SY, Xie YL, Yu ZH. Protection of Notoginseng polysaccharide on rat ischemia-reperfusion injury [J]. J Apopl Nerv Dis, 2015, 32(11): 996 998. [8] Ho YS, Yu MS, Yik SY, et al. Polysaccharides from wolfberry antagonizes glutamate excitotoxicity in rat cortical neurons [J]. Cell Mol Neurobiol, 2009, 29(8): 1233 1244. [9] Yang Y, Li W, Li Y, et al. Dietary Lyciumbarbarum polysaccharide induces Nrf2/ARE pathway and ameliorates insulin resistance induced by high-fat via activation of PI3K/AKT signaling [J]. Oxid Med Cell Long, 2014: 145641. doi: 10.1155/2014/145641. [10] Amagase H, Sun B, Borek C. Lyciumbarbarum (goji) juice improves in vivo antioxidant biomarkers in serum of healthy adults [J]. Nutr Res, 2009, 29(1): 19 25. [11] Chiu K, Chan HC, Yeung SC, et al. Modulation of microglia by wolfberry on the survival of retinal ganglion cells in a rat ocular hypertension model [J]. J Ocular Biol Dis Inf, 2009, 2(2): 47 56. [12],,,. [J]. (), 2016, 36(5): 661 665. Zhang YL, Huang XX, Huang ZR, et al. Study on the effects of Lyciumbarbarum polysaccharides (LBP) and LBP combined with tea polyphenols on relieving the physical fatigue in mice [J]. J Shanghai Jiaotong Univ (Med Sci Ed), 2016, 36(5): 661 665. [13] Zhu CP, Zhang SH. Lyciumbarbarum polysaccharide inhibits the proliferation of HeLa cells by inducing apoptosis [J]. J Sci Food Agric, 2013, 93(1): 149 156. [14]. [M]. :, 2015. Chinese pharmacopoeia commission. Pharmacopoeia of the people's republic of China 2015 edition, volume I [M]. Beijing: China Medical Science Press, 2015. [15],. [J]., 2016, 37(11): 143 146. Li L, Jin WJ. Comparative analysis on the determination methods of Lyciumbarbarum polysaccharide content [J]. Food Res Dev, 2016, 37(11): 143 146. ( 责任编辑 : 杨翠娜 )
6, : - 2271 作者简介 孔庆龙, 硕士, 主要研究方向为保健品 新食品开发 E-mail: 13238660658@163.com 游燕, 高级工程师, 主要研究方向为药物分析和质量研究 E-mail: yy81221@ynby-yimm.com 果蔬加工和质量安全控制专题 征稿函,,,,, (1) ( ); (2)( ); (3) ( ); (4) ; (5), 2017 10,,, 2017 9 30 Email 投稿方式 : : www.chinafoodj.com Email: jfoodsq@126.com 食品安全质量检测学报 编辑部