7 4 Vol. 7 No. 4 2016 4 Journal of Food Safety and Quality Apr., 2016 潘小红 1, 钟庆元 1, 刘玉玲 1, 周利平 (1., 410001; 2., 410001) 2* 摘要 : 目的 方法, 结果, 30 min,,, 518 nm 97.08%, 3.96%(n=9), 1, 8-0.0020~0.0252 mg/ml (r 2 =0.9996) 40~75 min 结论, 关键词 : ; ; ; 1, 8- Determination of total anthraquinones in health foods by ultraviolet pectrophotometry PAN Xiao-Hong 1, ZHONG Qing-Yuan 1, LIU Yu-Ling 1, ZHOU Li-Ping 2* (1. Hunan Institute for Food and Drug Control, Changsha 410001, China; 2. Hunan Science and Technology Exchange Center, Changsha 410001, China) ABSTRACT: Objective To establish a method for determination of total anthraquinone in health foods by ultraviolet pectrophotometry. Methods The methods for determination of total anthraquinones were optimized by studying on the instrument conditions, color stability, extraction methods, extraction solvents and hydrolysis acid choice and so on. Results Samples were extracted with mixed acid as extraction agent, with the direct heat reflux for 30 min, and then extracted by ether. Using mixed alkali to present color reaction, samples were detected at the wavelength of 518 nm. The average recovery of the detection was 97.08%, and the relative standard deviation (RSD) was 3.96%. 1, 8-dihydroxy anthraquinone had a good linear relationship at the range of 0.0020~0.0252 mg/ml (r 2 =0.9996), and samples could be measured within 40~75 min with good stability. Conclusion The established method has the advantages of simple operation, good stability and low cost, and is suitable for the determination of the content of total anthraquinone in health foods. KEY WORDS: total anthraquinone; health foods; ultraviolet pectrophotometry; 1,8-dihydroxy anthraquinone 1 引言 (anthraquinones), [1,2],, * 通讯作者 :,, E-mail: 284902963@qq.com *Corresponding author: ZHOU Li-Ping, Associate Research Fellow, Hunan Science and Technology Exchange Center, No. 59, Bayi Road, Furong District, Changsha 410001, China. E-mail: 284902963@qq.com
1626 7,, (2003 ), [3,4],,, [5], [6-17],,,, ~ (Borntrager ), ;,, [18-20],, 26 [21], (2015 ) 5 [22],,,, 1, 8-,,,, 2 材料与方法 2.1 实验材料 2015 11, 2.2 仪器与试剂 UV-2450 ( ); DG500 ( ) 1, 8- : 0829-9702,, 2.3 实验方法 2.3.1 标准溶液的配制 1, 8- : 1, 8-16.82 mg, 50 ml,, ( 0.3364 mg/ml) 1, 8- : l, 8-2 ml 10 ml,, 0 0.02 0.08 0.2 0.4 0.6 0.8 1.0 1.2 1.5 2.0 2.5 ml 10 ml, (10% 4% ),, 40 min,, 518 nm 2.3.2 仪器条件,, 190~900 nm, 2.3.3 样品前处理 : 0.1~1 g ( 0.0001 g); : 1~50 ml ( 0.01mL), 1~2 ml( ), 100 ml, (2 ml 25% +18 ml )10 ml, 30 min, ; 40 30 20 ml 3,,, ; 30 20 ml 2,, 50 20 20 ml 3,, 100 ml, (10% 4% ),, 40 min,, 30 min 2.3.4 呈色稳定性研究 0.8056 μg/ml 8.0560 μg/ml 25.1750 μg/ml 3, 5 min, 80 min 2.3.5 提取方式的选择 [6-17], 10 ml,,, 2.3.3 30min 2.3.6 水解酸的选择 (1)0.25 mol/l (2)2.5 mol/l (3)0.5 mol/l (4)5 mol/l (5) (2 ml 25% +18 ml )5,, 2.3.3 30min 2.3.7 萃取溶剂的选择,
4, : 1627 3 结果与分析 3.1 仪器及检测波长的选择 1, 8-190~900 nm 1,, 518 nm Fig. 2 2 1.8- Standard curve of 1, 8-dihydroxy anthraquinone 3.4 提取方式的选择 3.2 线性结果分析 1 1, 8- Fig. 1 Ultraviolet absorption spectrum of 1,8-dihydroxy anthraquinone (C), (A) 2, 1, 8-0.0020~0.0252 mg/ml 3.3 呈色稳定性考察 3, 40~75 min, ; 75 min,, 30 min,, 3 2,,, [20] 6, 4 4,, < < < < :,, ;,, 3.5 水解酸类型及浓度的选择 5,,, >, >, Fig. 3 3 1.8- Colour stability curves of 1, 8-dihydroxy anthraquinone
1628 7 3.6 萃取溶剂的选择, [2,4],,,,,, 0.7724 0.4123,, 3.7 回收率 Fig. 4 Fig. 5 4 Extraction effects of different extraction methods 5 Extraction effects of different acids hydrolysis, 9 ( 17.9752 mg/100 g), 3, 3, 1, 8- ( 0.3364 mg/ml)0.3 1.2 3.5 ml,, 1 3.8 样品测定, 6,,, 2 2,,,,,, 表 1 回收率结果 (n=9) Table 1 Results of recovery (n=9) (g) (mg) (mg) (mg) (%) (%) RSD(%) 5.0234 0.9030 0.1009 0.9988 95.00 97.08 3.96 5.1324 0.9226 0.1009 1.0156 92.24 4.9728 0.8939 0.4037 1.2762 94.70 5.0512 0.9080 0.4037 1.3040 98.10 5.0114 0.9008 1.1774 2.0799 100.14 5.0107 0.9007 1.1774 2.1050 102.29
4, : 1629 Fig. 2 表 2 样品测定结果对比 Comparison of the results of samples (mg/100g) (mg/100g) 1 0.85 0.88 2 0.63 0.64 3 45.23 57.14 4 102.94 110.72 5 42.99 50.77 6 1004 1022 4 讨论, 97.08%, 3.96%,,,,,,,,,,, 参考文献 [1],. [J]., 2009, 24(3): 237 238. Cao L, Zhou JJ. Research progress in the research of the compounds of the anthraquinone [J]. Northwest Pharm J, 2009, 24(3): 237 238. [2]. [C]. ( ), 2008: 172 174. Li JS. Analysis of the anhtraquinones, cytotoxicity and the potential safety risk of Chinese herbal medicine-containing health foods [C] Symposium on the analysis of medicinal plant chemistry and effective components of traditional Chinese Medicine (volume one), 2008: 172 174. [3] [EB/OL].(2016-01-01)http://cx.spsp.gov.cn/ index.aspx?token=$token$&first=first. National standard network [EB/OL]. [2016-01-01]. http://cx.spsp.gov.cn/index.aspx?token= $Token$&First =First. [4]. (2003 )[S]. The ministry of Health of the People's Republic of China. Health food inspection and evaluation of technical specifications(2003 Edition) [S]. [5]. [J]., 1998, 9(3): 188 189 Xiao HL. The restriction of the use of the anthracene compounds of plant laxative in Germany [J]. Tradit Chin Med Clin Harm, 1998, 9(3): 188 189 [6] Q/FSXHK0001J-2013 Q/FSXHK0001J-2013 Dian ao pai yi wei capsule, Beijing xinghuakang pharmaceutical technology Co., Ltd. enterprise standards [S]. [7] Q/BLW0003S-2012 [S]. Q/BLW0003S-2012 Li ren pai ni ke capsule, Wuhan century king biological engineering Co., Ltd. enterprise standards [S]. [8] Q/XAJC 0001S-2013 [S]. Q/XAJC 0001S-2013 Ai dong pai yin xing lu hui tea, Xi'an jiacheng pharmaceutical Co. Ltd. enterprise standard [S]. [9] Q/DXTJP 0079-2013 Q/DXTJP 0079-2013 Wu ji ren sheng oral liquid, Beijing tong ren tang health pharmaceutical limited by share Ltd enterprise standards [S]. [10] Q/XZS0002S-2012 Q/XZS0002S-2012 Yi li pai chang qing soft capsule, Xi'an zhengyuantang biology engineering Co., Ltd. enterprise standard [S]. [11] Q/RBH0010S-2012 Q/RBH0010S-2012 Bai he kang pai soft capsule, Rongcheng lily biotechnology Co., Ltd. enterprise standard [S]. [12] Q/AKJL0026S-2013 Q/AKJL0026S-2013 Bo wang pai sheng xi de bao capsule, Hunan jinliugu pharmaceutical Co., Ltd. enterprise standard [S]. [13] Q/CAXA004S-2013
1630 7 [S]. Q/CAXA004S-2013 Yan nong pai yin lan capsule, Hunan yan biological engineering co. ltd. enterprise standard [S]. [14] Q/SWJ 0142 S-2013. Q/SWJ 0142 S-2013 Nv ren yuan pai beauty-slimming tea, Food safety in Guangdong province enterprise standard [S]. [15] Q/KSW001-2008 Q/KSW001-2008 Lu ting pai lu ting slimming tea, Zunyi kang god biotechnology Co. Ltd. enterprise standard [S]. [16] Q/BKYY 0001S-2013 [S]. Q/BKYY 0001S-2013 San cao pai lu hui chang tong capsule, Guangxi boke pharmaceutical Co Ltd enterprise standard [S]. [17],,,. [J]., 2013, 34(5): 90 93. Huang Y, Wu Q, Wang X, et al. Content comparisons of total anthraquinones in weight-reducing tea [J]. Food Res Dev, 2013, 34(5): 90 93. [18]. [M]. :, 2006. Xu RS. Introduction to natural product chemistry [M]. Beijing: Science Press, 2006. [19],. [J]., 2005, 8(1): 24 27. Duan SE, Li M. Advances in the research of Chinese herbal medicine [J]. J Xi an Univ Arts Sci, 2005, 8(1): 24 27. [20]. ( )[M]. :, 2003. Wu LJ. Natural medicinal chemistry(4th Ed) [M]. Beijing: People's Medical Publishing House, 2003. [21]. [J]., 2006, 8(8): 27 30. Cai J. Functional components and health function of Aloe [J]. Food Med, 2006, 8(8): 27 30. [22]. ( )[M]. :, 2015. Chinese Pharmacopoeia Commission. Pharmacopoeia of the people's republic of china (Part one) [M]. Beijing: China Medical Science and Technology Publishing Press, 2015. 作者简介 ( 责任编辑 : 姚菲 ) 潘小红, 助理研究员, 主要研究方向为食品 药品 保健食品及化妆品的检验及研发 E-mail: panxiaohong56781@163.com. 周利平, 副研究员, 主要研究方向为科技成果推广 产业技术转移 科技金融等 E-mail: 284902963@qq.com