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    2015年, 第45卷, 第1期 刊出日期:2015-01-22 上一期    下一期
    基础研究
    一种含羟丙基的阳离子表面活性剂的流变性能
    Rheological performance of aqueous solution of a cationic surfactant containing hydroxypropyl group
    张旭东, 葛青, 李庆霞, 杨敏, 韩传红, 魏西莲
    2015 (1):  1-6.  doi: 10.13218/j.cnki.csdc.2015.01.001
    摘要 ( 298 )   PDF(3003KB) ( 346 )  
    用稳态和动态剪切流变学方法测定了3-十四烷氧基-2-羟丙基三甲基溴化铵(R14HTAB)水溶液的流变特性。结果表明,R14HTAB溶液的自组装结构在测定的浓度范围内经历了3次结构转变,从球形胶束到棒状胶束再到黏弹性的蠕虫状胶束,最后转变为六角状溶致液晶;在R14HTAB浓度超过360 mmol/kg以后为球形到棒状胶束的转变;交缠浓度约为500 mmol/kg,零剪切黏度(η0)与R14HTAB浓度(C)之间遵循指数关系,η0∝C5.7。用冷冻蚀刻电镜进一步证实了胶束的微观结构。稳态和动态黏度实验中Cox-Merz规律的偏离主要来自于氢键的形成。 Rheological performance of aqueous solution of a cationic surfactant (3-tetradecyloxy-2-hydroxypropyltrimethylammonium bromide,R14HTAB) was studied with steady and dynamic shear rheological method.Results showed that structure of the self-asembly of the R14HTAB undergoes three transitions in the shape within the investigated concentration range,from spherical to rodlike micelles,then to viscoelastic wormlike micelles,and finally to hexagonal lytropic liquid crystal.The transition from spherical micelles into rodlike micelles takes place as the concentration of R14HTAB higher than 360 mmol/kg.The overlapped threshold micelle concentration is about 500 mmol/kg.The viscosity at zero shear (η0) and R14HTAB concentration (C) displays exponential relationship,i.e.,η0∝C5.7.The microstructure of the formed micelles was further ascertained by FF-transmission electronic microscopy.The deviations from Cox-Merz rule in the steady and dynamic viscosity experiment is mainly due to formation of hydrogen bond.
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    科技讲座
    表面活性剂的性能与应用(XⅢ) ——表面活性剂的乳化作用及其应用
    Performance and applications of surfactants (XⅢ) Emulsifying action of surfactants and its applications
    张崴, 周雅文, 赵莉, 徐宝财
    2015 (1):  7-10.  doi: 10.13218/j.cnki.csdc.2015.01.002
    摘要 ( 465 )   PDF(785KB) ( 839 )  
    介绍了乳化作用的概念和乳状液的形成条件,简述了乳状液的基本性质、分类、鉴定方法及影响乳状液稳定性的因素,概述了如何选择乳化剂及HLB值的计算,介绍了乳化剂在农药、沥青、化妆品、食品和香料香精行业中的应用。 Concept with respect to emulsification and the conditions for emulsion formation were introduced.Basic properties,classification,appraising method and factors that affects stability of the emulsion were briefed.Way for selecting the emulsifier and calculation of HLB value were summarized.Applications of emulsifier in fields of pesticide,asphalt paving,cosmetics preparation,foods,fragrances and flavors were described.
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    开发与应用
    两性与氨基酸型阴离子表面活性剂形成自增稠体系的性质研究
    Study on properties of self-thickening system composed of amphoteric surfactant and amino-acid based anionic surfactant
    袁旻嘉, 董超, 沈珮琳, 卢海伟, 王进爽, 方波, 郭奕光
    2015 (1):  11-16.  doi: 10.13218/j.cnki.csdc.2015.01.003
    摘要 ( 509 )   PDF(2384KB) ( 882 )  
    通过调节质量比和pH,获得了由两性表面活性剂椰油酰胺丙基甜菜碱(CAPB)和氨基酸型阴离子表面活性剂月桂酰基肌氨酸钠(LS)复配的黏弹性胶束体系(自增稠体系)。通过低温冷冻透射电镜(Cryo-TEM)表征,确认了蠕虫状胶束结构。分析了NaCl含量对体系黏度的影响;着重考察了黏弹性体系的黏温性和发泡性。结果表明,NaCl含量(w<0.5%时)对该体系黏度影响较小,体系黏度的建立主要来自于质量比和体系pH;该体系在高温(40 ℃)时黏度降低,在低温(5 ℃)时黏度升高;当pH降低时,体系发泡性能变差。利用调节质量比和pH的方法,同时也能获得一系列氨基酸型阴离子表面活性剂和两性表面活性剂复配形成的自增稠体系,该方法具有一定的通用性。 A viscoelastic micelle system (self-thickening system) blended with an amphoteric surfactant,cocamidopropyl betaine (CAPB),and an amino-acid based anionic surfactant,sodium lauroyl sarcosinate (LS),was formed by adjusting the mass ratio and pH.The network of wormlike micelles in the blend was confirmed via characterization with Cryo-TEM images.Effect of NaCl dosage on the viscosity of the self-thickening system was identified and the viscosity-temperature characteristics as well as the foaming performance of the viscoelastic system were emphatically investigated.Results showed that when the NaCl content is low (w<0.5%) its effect on viscosity of the system is rather small.Establishment of viscosity of the system is mainly affected by mass ratio and pH of the system.The viscosity decreases at higher temperature (40 ℃) and increases at lower temperature (5 ℃),respectively.The foaming performance becomes worse as pH declines.Adopting the methods of adjusting the mass ratio and the pH,a series of self-thickening systems formed by blending of anionic amino-acid based anionic surfactant and amphoteric surfactant can be obtained.
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    阴香籽油合成单甘酯及其在润肤霜中的应用
    Synthesis of monoglycerides with Cinnamomum burmannii seed oil and its application in moisturizing cream
    董振浩, 刘光斌, 赵晓霞, 柳恒饶, 黄忠, 龚磊, 刘倩, 于伟伟
    2015 (1):  17-21.  doi: 10.13218/j.cnki.csdc.2015.01.004
    摘要 ( 350 )   PDF(794KB) ( 364 )  
    研究了甘油单阴香籽油脂肪酸酯的合成及其在化妆品中的应用。结果表明,阴香籽油酯交换合成甘油单酯的较佳条件为:醇油摩尔比为3∶1,催化剂NaOH的质量为油质量的0.8%,反应温度为180 ℃,反应时间为3 h,在此条件下合成的甘油单酯含量为62.6%。粗甘油单酯经分子蒸馏提纯,纯度可达92.8%。用此自制甘油单酯配制的润肤霜理化性能符合国家标准,使用性能较好,能够达到取代商品甘油单酯在润肤霜中的应用效果。 Synthesis of monoglycerides with Cinnamomum burmannii seed oil and its application in moisturizing cream were studied.The results showed that the optimal transesterification conditions of synthesis of monoglycerides with Cinnamomum burmannii seed oil were as follows:the glycerol to oil molar ratio of 3∶1;NaOH catalyst dosage of 0.8% of the oil mass;reaction temperature of 180 ℃ for 3 h;and the content reaches 62.6%.The crude product was purified by molecular distillation and the purity of the final product achieves 92.8%.Physicochemical properties of moisturizing cream prepared by using the final product can meet the requirements in China National Standard and the cosmetic product displays good performance in application.
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    钙皂分散剂十二烷基苄磺基甜菜碱与皂的复配性能研究
    Compatibility of lime soap dispersing agent N-dodecyl-N,N-dimethyl-N-(p-sulfobenzyl) betaine with soaps
    郑志辉, 胡学一, 方云
    2015 (1):  22-24.  doi: 10.13218/j.cnki.csdc.2015.01.005
    摘要 ( 288 )   PDF(784KB) ( 481 )  
    考察了钙皂分散剂N-十二烷基-N,N-二甲基-N-(p-苄磺基)甜菜碱(DSBB)与透明皂基的配伍性,测定了复配体系的抗硬水度、钙离子稳定性、去污力、泡沫性能、润湿性能和水溶温度。实验结果表明:由于DSBB的钙皂分散力高达3,在透明皂基中添加质量分数为10%的DSBB就能明显提高皂基的抗硬水性、去污力和润湿力;加入DSBB也有利于提高复配体系的低温水溶性,同时不会明显降低皂基的泡沫性能。 Compatibility of a lime soap dispersing agent,N-dodecyl-N,N-dimethyl-N-(p-sulfobenzyl) betaine (DSBB) with transparent soap base was investigated,and the performances of resistance to hard water,calcium tolerance,detergency,foaming power,wetting power and critical solution temperature were measured.Experimental results showed that lime soap dispersing power of DSBB was as high as 3.When the transparent soap was blended with 10% (mass fraction) of DSBB,the resistance to hard water,the detergency and the wetting power of the mixture were remarkably improved.DSBB was found beneficial to improve the solubility of the soap in cold water and without reducing the foaming power significantly.
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    十四烷基甲基二羟乙基溴化铵在织物上的性能研究
    Performance of myristylmethyldihydroxyethylammonium bromide on fabrics
    郑彩云, 高日成, 毛桃嫣, 黄颖红, 陈瑞兰, 赵朝晖, 郑成
    2015 (1):  25-27.  doi: 10.13218/j.cnki.csdc.2015.01.006
    摘要 ( 221 )   PDF(731KB) ( 325 )  
    研究了十四烷基甲基二羟乙基溴化铵作为衣物抗菌整理剂在棉布和无纺布中的抗菌、防霉和柔软性能。以不同质量浓度季铵盐处理过的棉布和无纺布做抗菌、防霉实验,得出该阳离子表面活性剂在质量浓度为1 000 mg/L时对大肠杆菌和金黄色葡萄球菌的杀菌效果显著,对黑曲霉、绳状青霉和球毛壳霉具有一定的抑制作用;通过对不同质量分数季铵盐处理过的棉布的柔软性能测试,表明质量分数为0.25%时柔软性能最佳。 Antibacterial,mould proof and softening performance of the quaternary ammonium salt myristyl-methyldihydroxyethylammonium bromide on cotton fabrics and non-woven cloth was studied. Via antibacterial and mould proof tests on cotton fabrics and non-woven cloth treated with the quaternary ammonium salt,results showed that,when the mass concentration of the quaternary ammonium salt achieves 1 000 mg/L,its effect is remarkable with respect to Escherichia coli and Staphylococcus aureus,while it displays certain inhibition effect on Aspergillus niger,rope Penicillium and spherical shell mold. Via cotton fabric softening tests with the quaternary ammonium salt of separate mass fractions,results showed that when the mass fraction achieves 0.25%,best softening effect can be obtained.
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    乳状液在储层中的注入性研究
    Study on injection of emulsions in reservoir bed
    徐金涛, 岳湘安, 宋伟新, 张德鑫, 苏群, 刘凯
    2015 (1):  28-31.  doi: 10.13218/j.cnki.csdc.2015.01.007
    摘要 ( 226 )   PDF(1314KB) ( 291 )  
    制备了一种稳定的水包油型乳状液体系,开展了此乳状液在30 cm长均质柱状岩芯的渗流实验,模拟乳状液在不同渗透率模拟储层中运移的过程。实验结果表明,平均粒径为3.673 μm的乳状液在渗透率0.6~1 μm2的岩芯中注入性和调驱能力都较好;当乳状液平均粒径与孔道平均直径的比值dr≤0.33时,乳状液的注入性较好,当dr>0.33时,随着dr的增大,乳状液的注入性迅速变差。 A kind of stable O/W emulsion was prepared in the laboratory.Seepage experiments of this emulsion in homogeneous cylindrical core with the length of 30 cm were carried out to simulate the seepage process of emulsion in reservoir beds with separate permeability.The experimental results showed that the emulsion with particles of 3.673 μm average diameter can be injected into deep of the core.In the cores with permeability from 0.6 to 1 μm2,the emulsion has good property both in profile control and injection.When the ratio of average diameter of emulsion and average diameter of core is less than 0.33,the property of injection is well.When the ratio of average diameter of emulsion and average diameter of core is larger than 0.33,as the ratio increases,the property of injection decreases quickly.
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    Fe3O4-ZnO复合材料的可控制备及其性能研究
    Controllable preparation and properties of Fe3O4-ZnO composites
    孙晶晶, 宋伟明, 孙立, 马帅, 刘鹏, 王斐
    2015 (1):  32-35.  doi: 10.13218/j.cnki.csdc.2015.01.008
    摘要 ( 232 )   PDF(3054KB) ( 338 )  
    采用水热-共沉淀法制备了Fe3O4-ZnO复合材料,利用SEM和XRD对Fe3O4-ZnO复合材料的微观结构进行了表征,并对复合材料的光催化性能和磁性能进行了研究。结果表明,制备的Fe3O4-ZnO复合材料的形貌可通过改变碱源的种类进行调控;光催化测试结果表明,当加入的碱源为NH3·H2O时制备出的Fe3O4-ZnO复合材料表现出优异的光催化活性,在100 min内对亚甲基蓝的降解率达到97.7%,重复使用3次后降解率仍达到96.5%。特别是这种材料具有很好的磁性(饱和磁化强度为25.881 A·m2/kg),可有效地对催化剂进行回收。 Fe3O4-ZnO composites were prepared with hydrothermal co-precipitation method.Microstructure of the composites was characterized by SEM and XRD.Photo-catalytic and magnetic performance were investigated.Experimental results showed that the morphology of the prepared Fe3O4-ZnO composites could be controlled and adjusted by changing the alkali source.Photo-catalysis test results indicated that the Fe3O4-ZnO composite prepared with NH3·H2O as alkali source displays excellent photo-catalytic activity,and the degradability of dye (methylene blue) using the composite achieves 97.7% within 100 min while after reuse of 3 times the degradability still achieves 96.5%.Notably,it displays good magnetic performance (saturated magnetization intensity achieves 25.881 A·m2/kg).Such materials can be effectively recovered and reclaimed.
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    负载玫瑰香精多孔微球的制备及缓释性能研究
    Preparation of porous microspheres encapsulated with rose fragrance and its slow-release performance
    苏忠毅, 裴广玲
    2015 (1):  36-40.  doi: 10.13218/j.cnki.csdc.2015.01.009
    摘要 ( 273 )   PDF(4861KB) ( 598 )  
    以分散聚合合成的单分散聚苯乙烯微球作为种子微球,采用两步种子溶胀法制备多孔聚苯乙烯-二乙烯苯微球,并吸附玫瑰香精制备了香精多孔微球。利用马尔文激光粒度仪、比表面积孔径分布测定仪(BET)、热重分析仪(TGA)、扫描电镜(SEM)对种子微球和多孔微球的粒径、比表面积和孔结构、缓释性能、表观形貌进行了分析表征。结果表明:种球的粒径随着分散介质中无水乙醇体积分数的增大而增加;随着溶胀剂邻苯二甲酸二丁酯(DBP)用量的增加,多孔微球的平均粒径变大,分布变宽;随着交联单体二乙烯苯(DVB)用量增加,多孔微球平均粒径减小,分布变窄;以甲苯为致孔剂制备的多孔微球单分散性最好。当V(DBP)∶m(种球)=3∶1,V(DVB)∶V(苯乙烯)=4∶0时,制备的多孔微球的平均粒径约为4 μm。以此多孔微球负载玫瑰香精,可以减缓香精的释放速率,提高起始分解温度,实现对香精的缓释。 Porous microspheres encapsulated with rose fragrance were prepared by adsorption of the fragrance on porous polystyrene-divinylbenzene (PSt-DVB) microspheres,which were obtained by two-step swell polymerization with the uniform polystyrene microspheres as seed particles via dispersion polymerization.The surface features of seed particles and porous microspheres were observed by scanning electron microscope (SEM);the particle size,the specific surface area and pore structure were analyzed and characterized by particle size analyzer and Brunauer,Emmett and Teller (BET) method;controlled-release performance was tested by thermal gravimetric analysis (TGA).The results showed that the particle size of the seed particles increases with the increasing of volume fraction of the ethanol.As dosage of the swelling agent,p-dibutyl phthalate (DBP) increases,particle size of the porous microspheres increases and its distribution becomes wider.As the dosage of cross-linking monomer DVB increases,average particle size of the porous microspheres reduces and its distribution becomes narrower.The best single size dispersion was obtained as the porous microspheres were generated with toluene.The porous PSt-DVB microspheres with the diameter of 4 μm were obtained when the ratio of V(DBP)∶m(seed particles) and V(DVB)∶V(St) is 3∶1 and 4∶0,respectively.As a result,the release rate of the fragrance can be slow down and initial decomposition temperature can be raised;and then the controlled release of the fragrance can be realized.
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    p-茴香酸与脱水山梨醇辛酸酯的复配物在洗发香波中的应用研究
    Application of blend of p-anisic acid and sorbitan caprylate in hair shampoo
    汪冰洁, 张怡, 龚盛昭
    2015 (1):  41-44.  doi: 10.13218/j.cnki.csdc.2015.01.010
    摘要 ( 354 )   PDF(798KB) ( 480 )  
    采用防腐挑战测试方法研究了p-茴香酸与脱水山梨醇辛酸酯作为防腐剂在洗发香波中的抑菌性能。对其用量及抑菌条件(体系pH和温度)对抑菌效果的影响进行了考察,结果表明,当p-茴香酸的质量分数为0.4%,脱水山梨醇辛酸酯的质量分数为1.0%,且体系pH≤6.0时,体系具有良好的抑菌性能。 Bacterial inhibitory performance of blends of p-anisic acid and sorbitan caprylate in hair shampoo was studied by preservation test method. Effect of dosage of the antibacterial agents,as well as the application conditions (pH and temperature of the system) on inhibition result was examined. Results showed that as the mass fraction of the p-anisic acid achieves 0.4% and the sorbitan caprylate achieves 1.0%,as well as the pH keeps no more than 6.0,the system displays good antibacterial performance.
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    四物汤美白功效评价及其药效关系研究
    Study on the whitening efficacy of Siwu-tang and the relationshipwith its pharmacodynamic function
    尤卓莹, 何秋星, 李馨恩, 黄永红, 林春雨
    2015 (1):  45-48.  doi: 10.13218/j.cnki.csdc.2015.01.011
    摘要 ( 315 )   PDF(784KB) ( 493 )  
    利用水提法提取四物汤,采用DPPH(1,1-二苯基-2-三硝基苯肼)分析法测定四物汤的抗氧化活性,用紫外分光光度法测定四物汤对酪氨酸酶的抑制作用,综合评价四物汤的美白功效。同时以对DPPH自由基的清除率和对酪氨酸酶的抑制率为评价指标,运用均匀设计法研究四物汤剂量比例与美白功效的关系。结果表明,用水提法提取的四物汤具有较强清除DPPH自由基的能力,对酪氨酸酶活性呈高质量浓度抑制,低质量浓度激活的作用。均匀设计实验中,当四物汤采用m(当归)∶m(川芎)∶m(白芍)∶m(熟地)=85∶66∶10∶199时,对酪氨酸酶活性的抑制率为24.3%,对DPPH自由基的清除率为95.2%,具有较好的美白效果。 Siwu-tang was prepared by water extraction of four kinds of Chinese traditional herb medicine.DPPH (1,1-diphenyl-2-picryl-hydrazyl) method was adopted to measure the antioxidant activity of the Siwu-tang and ultraviolet spectrophotometry was adopted to measure the tyrosinase inhibitory activity.Then the whitening efficacy of Siwu-tang was comprehensively evaluated.Meanwhile,taking DPPH free radical scavenging ratio and tyrosinase inhibitory ratio as assessment indices,as well as adopting uniform design method,the relationship between dosage ratio of the Siwu-tang and the whitening efficacy was investigated.Results showed that,the Siwu-tang displays rather high DPPH free radical scavenging capacity.With respect to activity of tyrosinase,it displays inhibitory action at high mass concentration,while at lower mass concentration it displays activation effect.In the uniform designed experiment,the results showed that when the mass ratio in the composition of the Siwu-tang Radix Angelica sinensis,Rhizoma Chuanxiong,Radix Paeoniae Alba and Radix Rehmanniae Praeparata is 85∶66∶10∶199,the inhibitory ratio of tyrosinase activity achieves 24.3%,and the scavenging ratio of DPPH free radicals achieves 95.2%.
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    分析与检测
    高效液相色谱法测定染发剂中32种禁限用染料
    Determination of 32 kinds of banned and/or restricted dyestuff in hair dyes by high performance liquid chromatography
    严巍, 胡磊, 周明昊
    2015 (1):  49-54.  doi: 10.13218/j.cnki.csdc.2015.01.012
    摘要 ( 360 )   PDF(853KB) ( 410 )  
    建立了染发剂中32种禁限用染料含量的反相高效液相色谱测定方法。根据每个化合物的pKa将32种物质分成3组,采用ZORBAX Extend C18 (4.6 mm×250 mm,5 μm)和ZORBAX Bonus-RP C18 (4.6 mm×250 mm,5 μm)色谱柱,以甲醇、乙腈和pH分别为7.0,8.0和9.0的缓冲盐溶液作为流动相,在流速为1.0 mL/min,检测波长分别为280,230和250 nm的条件下进行测定。结果表明,相对标准偏差均小于5%,加标回收率为70%~130%。 A reversed phase high performance liquid chromatography (HPLC) method was established for the determination of 32 kinds of banned and/or restricted dyestuff in hair dyes.The 32 kinds of dyestuff were divided into three groups according to the value of pKa of each component.ZORBAX Extend C18 (4.6 mm×250 mm,5 μm) column and ZORBAX Bonus-RP C18 (4.6 mm×250 mm,5 μm) column were used.Methanol,acetonitrile and buffer salts with pH of 7.0,8.0 and 9.0 respectively were used as the mobile phase.The flow rate was 1.0 mL/min and the detection wavelengths were 280,230 and 250 nm respectively.All the RSD values are lower than 5%.The spiked recovery achieves 70% to 130%.
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    正相高效液相色谱法同时测定化妆品中2种熊果苷含量
    Simultaneous determination of α-,β-arbutin in cosmetics by normal phase high performance liquid chromatography
    张乐, 王卫华, 姜艳艳, 杨元, 刘斌
    2015 (1):  55-59.  doi: 10.13218/j.cnki.csdc.2015.01.013
    摘要 ( 227 )   PDF(791KB) ( 304 )  
    采用正相高效液相色谱,建立了化妆品中α-,β-熊果苷的含量测定方法。采用S-Chiral A色谱柱(250 mm×4.6 mm,5 μm)和二极管阵列检测器,以V(正己烷)∶V(乙醇)=70∶30的混合溶液为流动相,流速为0.8 mL/min,检测波长为226 nm,柱温为30 ℃。α-,β-熊果苷的检出限(S/N=3)分别为1.5和3.6 ng,定量限(S/N=10)分别为1.6和6.3 ng,10~500 mg/L内,峰面积与质量浓度呈良好的线性关系,相关系数分别为1.000 0和0.999 0。高、中、低不同水平的加标回收率为99.61%~103.36%,RSD不大于0.80% (n=6)。该方法操作简便,准确度、灵敏度和稳定性高,可用于化妆品中α-,β-熊果苷的含量测定。 An analysis method was established for determination of α-,β-arbutin in cosmetics by normal phase high performance liquid chromatography. The separation was performed on an S-Chiral A column (250 mm×4.6 mm,5 μm) with n-hexane-ethanol (volume ratio 70∶30) as the mobile phase at a flow rate of 0.8 mL/min. The detection wavelength was 226 nm. Operating temperature was 30 ℃. The limit of detection of α-,β-arbutin are 1.5 and 3.6 ng respectively,and the limit of quantification are 1.6 and 6.3 ng respectively. A good linear relationship is obtained between the peak area and the mass concentration of α-,β-arbutin in the range of 10~500 mg/L and the correlation coefficient are 1.000 0 and 0.999 0 respectively. The recoveries of α-,β-arbutin at different spiked level are 99.61%~103.36% with the relative standard deviations (RSD) no more than 0.80%.
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