40 9 Journal of South China University of Technology Vol 40 No 9 2012 9 Natural Science Edition September 2012 1000-565X 2012 09-0032-06 * 5 510640 5 ph SDS 15 mmol /L 30 mmol /L SDS 10% ph 9 6 25 kv 5 18 min 1 06% ~ 1 61% 1 46% ~ 2 87% 0 26 ~ 0 56 mg /L 97 2% ~ 103 2% TQ041 + 7 R284 1 doi 10 3969 /j issn 1000-565X 2012 09 006 Polygonum multiflorum Thunb 1 20 80 2-3 2 3 5 4'- -2-O-β-D 4 2010 CMC 5 5 6 1 7-8 9-11 4 12-14 1 5 1 1 P /ACE TM MDQ 2012-03-26 * 31071559 NCET-11-0161 1971- E-mail bbhwu@ scut edu cn
9 5 33 Beckman ph 32 Karat 7 0 ph 8 8 57 0 cm 75 0 μm i d 50 0 cm ph 8 8 9 6 CP-225D PB-10 ph ph ph 9 6 Sartorius ph 9 6 ph 9 6 SDS Alfa Aesar 1 2 100 mmol /L SDS ph - SDS- 4 00 mg 10 ml 400 mg /L 4 Fig 1 Effect of of buffer solution ph value on separation of 100 200 0 mg 50 ml stilbene glucoside and five anthraquinones 15 min 10 ml 2 10 ml 1 3 MECC 10 min 2 0 1 mol /L SDS 2 10 min 2 0 1 mol /L SDS 10 ~ 50 mmol /L 10 min 2 min SDS SDS 0 1 mol /L 0 1 mol /L 20 mmol /L 5 min 2 min 0 5 PSI 10 s 254 nm 25 60% 2 2 1 10 4 1 1 ph 5 10% CH 3 OH 20 kv 2 1 2 SDS 2 1 1 ph 2 SDS 5 ph Fig 2 Effect of SDS concentration on separation of stilbene ph glucoside and five anthraquinones 15 mmol /L Na 2 B 4 O 7 SDS 10% CH 3 OH 5 ph 9 6 20 kv
34 40 SDS 30 mmol /L 10% SDS 30mmol /L SDS 30 mmol /L 2 1 3 3 15 mmol /L 4 5 15 mmol /L Fig 4 Effect of methanol concentration on separation of stilbene glucoside and five anthraquinones 15 mmol /L CH 3 OH ph 9 6 20 kv 15 mmol /L 2 1 5 15 15 ~ 25 kv 25kV 25 kv 3 5 15mmol /L 30mmol /L SDS 10% ph Fig 3 Effect of Na 2 B 4 O 7 concentration on separation of stilbene glucoside and five anthraquinones 50 mg /L 9 6 25kV 6 5 18 min Na 2 B 4 O 7 30 mmol /L SDS 10% CH 3 OH ph 9 6 20 kv 2 1 4 5 MECC 0 ~ 20% 5 5 4 Fig 5 Electrogram of stilbene glucoside and five anthraquinones under the optimum capillary electrophoresis 5% 15% conditions 10% CH 3 OH ph 9 6 25 kv
9 5 35 2 2 6 2 5 50 mg /L 97 2% ~ 103 2% 6 RSD 1 06% 1 31% 1 61% 1 51% 1 35% 1 15% RSD 1 46% 1 69% 1 94% 2 01% 2 87% 2 53% 6 5 S /N = 3 1 Fig 6 Electrogram of stilbene glucoside and five anthraquinones in Polygonum multiflorum Thunb sample 1 5 S /N = 3 Table 1 Linear regression equations linear correlation coefficients linear ranges and detection limits S /N = 3 of stilbene glucoside and five anthraquinones / / mg L - 1 mg L - 1 y = 356 7x + 4362 8 0 994 3 5 ~ 400 0 26 y = 1026 1x + 47293 3 0 9926 5 ~ 200 0 44 y = 1197 5x + 44102 4 0 9953 5 ~ 200 0 35 y = 4 082 1x - 1 596 5 0 9942 5 ~ 200 0 38 y = 1692 8x + 42930 8 0 9946 5 ~ 100 0 43 y = 2502 2x + 28403 0 0 9916 5 ~ 100 0 56 2 3 5 2 5 100 18 min 200 mg 400 /L 0 26 ~ 0 56 mg /L 97 2% ~ 103 2% 1 2 2 Table 2 Component analysis results of sample and recoveries / / RSD /% /mg /% mg g - 1 mg g - 1 12 02 1 20 17 77 98 6 1 6 2 16 0 40 4 21 101 2 1 9 1 16 0 20 2 21 102 1 2 4 1 00 4 92 98 4 2 9 0 58 0 15 1 29 97 2 3 1 0 50 2 58 103 2 2 7 10% CH 3 OH ph 9 6 25 kv 5 13 20 min 18 min 3 1 J 2000 5 326-328 Guo Qing Lu Jing HPLC determination of anthraquinone in Radix polygoni multiflori and Radix polygoni multiflori preparata J Chinese Journal of Pharmaceutical Analysis 2000 20 5 326-328
36 40 2000 16 3 151-154 Yuan Hai-long He Cheng-shan Xiao Xiao-he et al De- 2 J termination of stilbene in Polygonum multiflorum Thunb 2010 29 1 72-75 by capillary electrophoresis J Pharmaceutical Journal of Tan Kai-li Liao Hai-min The advances in pharmacological effects in Polygonum multiflorum J Journal of Mountain Agriculture and Biology 2010 29 1 72-75 3 electrophoresis with beta-cyclodextrin addition J Journal of Chromatography A 2006 J 2008 26 8 1687-1123 134-137 1689 Han Xiao Wu Cheng-ai Wang Wei et al Mechanism research of stilbene glucoside from Polygonum multiflorum Thunb on hyperlipemia J Chinese Archives of Traditional Chinese Medicine 2008 26 8 1687-1689 4 Zhang F Chen W S Sun L N LC-VWD-MS determination of three anthraquinones and one stilbene in the quality control of crude and prepared roots of Polygonum multiflorum Thunb J Chromatographia 2008 67 11 /12 1277-1280 Wang Yu-xia Liu Bin Shi Ren-bing et al Research on quality control method of stilbene fraction of Polygonum multiflorum Thunb J China Journal of Traditional Chinese Medicine and Pharmacy 2009 24 10 1277-1280 Thunb by TLCS J Science and Technology of Food Industry 2008 29 9 271-272 7 HPLC J 2010 17 18 41-42 Su Li-jie HPLC determination of stilbene glucoside in Polygonum multiflorum content determination of content of 2 3 5 4'-tetrahydroxystilbene-O-β-D-glucoside in Radix polygoni multiflori J China Modern Medicine 2010 17 18 41-42 8 HPLC Radix polygoni muliflori by micellar electrokinetic capillary chromatography J Journal of Hebei University J 2009 24 3 285-287 of Liu Yan Chao Ruo-bing Determination of two anthraquinones in different Polygonum multiflorums by HPLC J West China Journal of Pharmaceutical Sciences 2009 24 3 285-287 9 Yang Gui-di Zheng Jin-ping Huang Hong-xia et al J Speciation analysis of arsenic in sea foods with capillary Chinese People s Liberation Army 2000 16 3 151-154 10 Tian K Zhang H G Chen X G et al Determination of five anthraquinones in medicinal plants by capillary zone 11 J 2006 22 1 68-70 Li Wei Chai Jin-ling Alimjan Abaydulla et al Separation and determination of anthraquinone compounds in Chinese herb Rhubarb extracts by capillary zone electrophoresis J Journal of Analytical Science 2006 22 1 68-70 12 869-874 J 2007 18 8 1934-5 1935 J 2009 24 10 Chen Xiao-ying Yan Han-jing Fu Jun Quality evaluation of Radix polygoni multiflori from different areas by TLC-fingerprint J Lishizhen Medicine and Materia Medica Research 2007 18 8 1934-1935 13 HPLC 5 J 6 J 2012 27 2 463-465 2008 29 9 271-272 Zhu Pei-fang Zhao Rong-hua Shi Yang-xian Determina- Zhang Xue Analysis of emodin in Polygonum mutiflorum tion of stilbeneglycoside and 5 kinds of anthraquinone in Polygonum multiflorum Thunb by HPLC stimultaneously J China Journal of Traditional Chinese Medicine and Pharmacy 2012 27 2 463-465 14 J 2011 32 5 426-430 Wu Xian Chen Guan-hua Wang Kun et al Determination of stilbene glycoside emodin and chrysophanol in Science and Technology 2011 32 5 426-430 15 J 2009 37 4 532-536 electrophoresis-ultraviolet detection J Chinese Journal of Analytical Chemistry 2009 37 4 532-536
9 5 37 Simultaneous Determination of Stilbene Glucoside and Five Anthraquinones in Polygonum multiflorum Thunb by Means of Micellar Electrokinetic Capillary Chromatography Wu Hong Wang Yan Wen Peng Lou Wen-yong Zong Min-hua School of Light Industry and Food Sciences South China University of Technology Guangzhou 510640 Guangdong China Abstract In this investigation a method of using the micellar electrokinetic chromatography was laid down for the simultaneous determination of stilbene glucoside and five anthraquinones including emodin aloe-emodin rhein chrysophanol and physcion in Polygonum multiflorum Thunb and the effects of the buffer solution ph value the SDS concentration the sodium tetraborate concentration the methanol volume fraction and the operating voltage on the separation and determination were discussed The results show that optimal separation and determination conditions are an operating voltage of 25 kv and a buffer solution with a ph value of 9 6 15 mmol /L of sodium tetraborate 30 mmol /L of SDS and 10% volume fraction of methanol and that in the optimal conditions stilbene glucoside and the five anthraquinones are completely separated within 18 minutes with a relative standard deviation of migration times of 1 06% ~ 1 61% a relative standard deviation of peak areas of 1 46% ~ 2 87% a detection limit of 0 26 ~ 0 56 mg /L and a recovery of 97 2% ~ 103 2% Key words micellar electrokinetic capillary chromatography Polygonum multiflorum Thunb stilbene glucoside anthraquinones 31 Effects of Binder Resins on Expansion and Flame-Retardant Performances of Waterborne Fire-Retardant Coatings Fan Fang-qiang Xia Zheng-bin Li Qing-ying Li Zhong Chen Huan-qin School of Chemistry and Chemical Engineering South China University of Technology Guangzhou 510640 Guangdong China Abstract In this investigation the waterborne ultra-thin fire-retardant coatings for steel structures were prepared respectively with the silicone-acrylic acrylic styrene-acrylic and VAc-VeoVa latexes as the binder Then the effects of the binders on the fire-retardant performance of the coatings were discussed in terms of the thermal stability and the high-temperature rheology The combustion test results of analoging large panels show that the expansion ratio 17 4 times that of the fire-retardant coatings from the VAc-VeoVa latex is the largest and its fire-retardant performance is the best with a steel backside temperature of 304 after a 30-min combustion It is seen from TGA curves that the VAc-VeoVa polymer is of good thermal stability and its average thermal degradation rate is the lowest and that those characteristics of the VAc-VeoVa polymer provide enough time for its reaction with ammonium polyphosphate thus generating a dense char layer which can remarkably improve the fire-retardant performance of the coating Moreover the results of the dynamic rheological test demonstrate that for the acrylic and styreneacrylic molten polymers the storage modulus G' are higher than the loss modulus G which means that the elastic flow is predominant in these melts and their complex viscosities are more than 1 000 Pa s while for the VAc-VeoVa molten polymer G is higher than G' which means that the viscous flow is predominant in this melt and its complex viscosity is 33 Pa s and that for the VAc-VeoVa melt a Newtonian fluid property is displayed at the low frequency stage and the complex viscosity slightly decreases at the end of the high frequency stage The above-mentioned results show that the viscous fluid with good thermal stability and low complex viscosity can be used as the binder of fire-retardant coatings which is helpful in the expansion and fire retardancy of the coatings Key words waterborne ultra-thin fire-retardant coating binder dynamic rheological property fire-retardant performance