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2015年, 第45卷, 第4期　刊出日期：2015-04-22 上一期    下一期

基础研究

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脂肪醇聚氧乙烯醚羧酸钠与双癸基羟乙基甲基氯化铵复配性能研究 Study on the properties of blend system of sodium fatty alcohol ether carboxylate and bis-decylmethylhydroxyethylammonium chloride 刘晓英, 台秀梅, 杜志平, 王国永, 赵慧贤, 王天壮 2015 (4):  181-184.  doi: 10.13218/j.cnki.csdc.2015.04.001 摘要 ( 307 )   PDF(1519KB) ( 368 )   分别采用表面张力仪、紫外-可见分光光度计和透射电子显微镜(TEM)测试了脂肪醇聚氧乙烯醚羧酸钠(AE9C)与双癸基羟乙基甲基氯化铵(DEQ)复配体系的表面性能、稳定性和聚集行为。结果表明,复配体系具有明显的协同增效作用,当AE9C与DEQ的质量比为4∶6时,表面的饱和吸附量达到最大(2.15×10-10 mol/cm2),极性头基所占的截面积最小(0.77 nm2),表面活性最强;复配体系具有很好的稳定性,AE9C与DEQ的质量比大于5∶5时,即使质量分数为10.0%也能形成稳定透明的溶液,且放置1个月不分层;AE9C与DEQ的质量比为4∶6,质量分数为4.0%时,形成的溶液具有一定的黏度,TEM测试发现溶液中存在无规排列的规则棒状聚集体。 Surface activity,stability and aggregation behavior of blend systems of sodium fatty alcohol ether carboxylate (AE9C) and bis-decylmethylhydroxyethylammonium chloride (DEQ) were measured by surface tensiometer,UV-Vis spectrophotometer and transmission electron microscopy (TEM),respectively.Results showed that the blend system that displays best synergistic effect is at the mass ratio of m(AE9C)∶m(DEQ)=4∶6,which displays Γmax=2.15×10-10 mol/cm2,Amin=0.77 nm2.The blend system shows very excellent stability.When the mass ratio of AE9C and DEQ is bigger than 5∶5,even if the mass concentration achieves 10.0%,uniform and stable solutions are formed and the solutions can keep its homogeneity without stratification after a month.When the mass fraction is 4.0% with m(AE9C)∶m(DEQ)=4∶6,a solution with fixed viscosity is formed and TEM test results depicted random arrangement of rod-like aggregates. 参考文献 | 相关文章 | 计量指标

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Ugi反应海藻酸衍生物协同疏水改性高岭土稳定Pickering乳液的制备 Preparation of stable Pickering emulsions by alginate derivative prepared via Ugi reaction in cooperation with hydrophobically modified kaolin 陈秀琼, 颜慧琼, 李嘉诚, 冯玉红, 史载锋, 王向辉, 林强 2015 (4):  185-190.  doi: 10.13218/j.cnki.csdc.2015.04.002 摘要 ( 223 )   PDF(2044KB) ( 317 )   通过Ugi反应疏水改性海藻酸钠(Alg),制备了两亲性的海藻酸衍生物(Ugi-Alg)。以聚甲基氢硅氧烷(PMHS)作为疏水改性剂,利用干法球磨对高岭土(KL)微粒表面疏水改性。并利用FTIR、1HNMR、接触角测量仪、激光粒度和Zeta电位分析仪对改性产物进行表征。用改性后的高岭土(MKL)协同Ugi-Alg制备稳定的Pickering乳液,并探究了水相pH对Pickering乳液形貌和液滴大小的影响。结果表明:Alg通过Ugi反应成功地疏水改性;PMHS在球磨的机械作用下吸附在KL微粒表面,使MKL成为具有高疏水性能的活性微粒;Ugi-Alg在超声作用下协同吸附在MKL微粒表面,改变了MKL微粒表面的润湿性,可提高Pickering乳液的稳定性;随着水相pH的升高,MKL/Ugi-Alg稳定的Pickering乳液液滴粒径逐渐减小,当pH=10.32时,其液滴粒径达到7.4 μm。 Amphiphilic alginate derivative (Ugi-Alg) was prepared via Ugi reaction of hydrophobically modified sodium alginate (Alg).The kaolin (KL) particle's surface was hydrophobically modified with dry ball milling method,using poly (methyl hydrosiloxane) (PMHS) as hydrophobic modifying agent.Then the properties of the modified products were characterized by FTIR,1HNMR,contact angle measurement,laser particle size measurement and Zeta potential analyzer.The stable Pickering emulsions were prepared by the modified kaolin (MKL) in cooperation with Ugi-Alg and effects of pH of the water phase on the morphological characteristics and the emulsions' droplet size of the Pickering emulsions were investigated.Experimental results showed that the hydrophobic modification of Alg by Ugi reaction is successful.PMHS is adsorbed on the surface of KL under the mechanical action of the ball milling,making MKL become the active particle with high hydrophobic property.Ugi-Alg is coordinately adsorbed on the particle's surface of MKL under action of ultrasonic wave,changing the wettability of MKL particles' surface,which could effectively improve the stability of the Pickering emulsions.As the raising of pH of the water phase,droplet size of the MKL/Ugi-Alg Pickering emulsions is gradually declined.When the pH achieves 10.32,the emulsions' droplet size reaches 7.4 μm. 参考文献 | 相关文章 | 计量指标

科技讲座

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表面活性剂的性能与应用(XVI)——表面活性剂在食品工业中的应用 Performance and applications of surfactants (XVI) Applications of surfactants in food industry 胡俊, 刘红芹, 徐宝财, 赵莉 2015 (4):  191-195.  doi: 10.13218/j.cnki.csdc.2015.04.003 摘要 ( 394 )   PDF(884KB) ( 569 )   从表面活性剂的结构和性质出发,论述了表面活性剂作为食品乳化剂、增溶剂、起泡和消泡剂及增稠剂等的作用机理,概述了表面活性剂在食品工业中的应用,并对可食用表面活性剂的发展和应用进行了展望。 Based upon the structure and applications of surfactant,the functional mechanism of surfactant which was used as food emulsifiers,solubilizers,foaming and defoaming agents as well as thickeners were reviewed.Meanwhile,the applications of surfactants in the food industry were summarized.The development and future applications of edible surfactants were prospected as well. 参考文献 | 相关文章 | 计量指标

开发与应用

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撞击流-旋转填料床制备丙烯酰胺反相乳液及其稳定性研究 Preparation and stability of acrylamide inverse-phase emulsion with impinging stream-rotating packed bed reactor 李小月, 张巧玲, 李磊, 魏冰, 刘有智 2015 (4):  196-200.  doi: 10.13218/j.cnki.csdc.2015.04.004 摘要 ( 309 )   PDF(1059KB) ( 422 )   以撞击流-旋转填料床为乳化设备,煤油为有机介质,山梨醇酐油酸酯(Span 80)和烷基酚聚氧乙烯醚(OP-10)为复配乳化剂制备了丙烯酰胺反相乳液,研究了超重力因子、撞击速度、油水体积比、乳化剂质量分数、复配乳化剂HLB值以及丙烯酰胺单体质量分数对乳液稳定性的影响,并与搅拌式乳化装置进行了对比研究。结果表明:在超重力因子为65.32,撞击速度为12.58 m/s,V(油相)∶V(水相)=1∶1,乳化剂质量占乳液总质量的5%,复配乳化剂HLB值为6.0,丙烯酰胺单体质量占单体水溶液总质量的15%的条件下,所制备乳液平均粒径为664 nm,稳定性系数达0.973;对比研究发现,采用撞击流-旋转填料床制备的乳液稳定性好,粒径小,分散均匀,乳化时间短,为连续化制乳过程。 Acrylamide inverse-phase emulsion was prepared with kerosene as organic medium,sorbitan monooleate (Span 80) and alkylphenol polyoxyethylene ether (OP-10) as blended emulsifier,as well as impinging stream-rotating packed bed reactor as emulsification equipment.Effect of super gravity factor,impinging speed,volume ratio of oil to water,mass fraction of emulsifier,HLB value of the blended emulsifier and mass fraction of acrylamide monomer content on stability of the emulsion was studied.Comparison was made with that obtained with stirring emulsification device.Results showed that at the conditions of 65.32 super gravity factor;12.58 m/s impinging speed;1∶1 volume ratio of oil to water;5% mass fraction of emulsifier in total emulsion;6.0 HLB value of the blended emulsifier and mass fraction 15% of acrylamide monomer in water solution,the average emulsion particle size of the emulsion achieves 664 nm,and stability coefficient can achieve 0.973.Comparison study showed that stability,particle size and dispersion of emulsion prepared with impinging stream-rotating packed bed reactor is better,emulsification time is shorter,and the preparation process of the emulsion is continuous. 参考文献 | 相关文章 | 计量指标

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十六烷基三甲基溴化铵为模板剂在水/丙酮介质中合成纳米SiO2空心球 Fabrication of SiO2 nano-hollow spheres with CTAB as template agent in water-acetone media 张金昌, 石磊, 郭新闻, 刘兆滨, 朱建民 2015 (4):  201-205.  doi: 10.13218/j.cnki.csdc.2015.04.005 摘要 ( 276 )   PDF(1281KB) ( 329 )   在水和丙酮的混合介质中,当1<n(水)/n(丙酮)<15时,以十六烷基三甲基溴化铵为模板剂,合成出介孔实心球;再用正丁胺为模板剂,通过水热法合成出具有微孔结构的纳米SiO2空心球。结果表明,当晶化时间为48 h时,所得空心球的直径为600～800 nm,空心球的球壳厚度约70 nm,孔径约为0.47 nm。 Mesoporous solid spheres were synthesized in water-acetone media using cetyltrimethylammonium bromide as the template agent under condition of water-to-acetone molar ratio lying between 1 and 15.Then SiO2 nano-hollow spheres with micropore structure were synthesized from the mesoporous solid spheres by hydrothermal treatment with n-butylamine as template agent.Results showed that the solid spheres are converted into hollow spheres in crystallization time of 48 h,and diameter of the hollow spheres lying between 600 and 800 nm in size with shell thickness of ca.70 nm and pore size of ca.0.47 nm. 参考文献 | 相关文章 | 计量指标

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植物油型防结块剂的制备条件研究 Preparation of anti-caking agent using vegetable oil as raw material 薛源, 张丽, 程亮, 张保林 2015 (4):  206-209.  doi: 10.13218/j.cnki.csdc.2015.04.006 摘要 ( 302 )   PDF(812KB) ( 456 )   以植物油、非铵盐类表面活性剂为原料,制得一种环境友好型防结块剂,通过模拟堆压加速结块法对施用该防结块剂复混肥的防结块效果进行了测定。结果表明,当m(防结块剂)∶m(复混肥)=5∶1 000,防结块剂组成为m(聚乙二醇2000+聚二甲基硅氧烷)∶m(聚山梨酯B)=1∶2且m(复配表面活性剂)∶m(植物油)=1∶100时,复混肥的最小结块率可达到9.0%,优于机油-胺类防结块剂。 An environmentally friendly anti-caking agent product was prepared with vegetable oil and non-ammonium salt surfactant as raw materials.Anti-caking efficacy of the product was tested by accelerated compression stacking simulation method.Test results showed that in case the mass ratio of the materials is m(anti-caking agent product)∶m(blended fertilizer)=5∶1 000,and mass ratio for composition of the anti-caking agent product is m(PEG 2000+PDMS)∶m(polysorbate B)=1∶2 and m(blended surfactants)∶m(vegetable oil)=1∶100,the caking ratio achieves the lowest as 9.0%,which is better than that of conventional anti-caking agents made of machine oil and ammonium compounds. 参考文献 | 相关文章 | 计量指标

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相转移催化合成4,4′-二羧基二苯甲酮 Synthesis of 4,4′-dicarboxylbenzophenone with phase transfer catalysis 张彦杰, 蒋文伟, 杨琴, 罗芩 2015 (4):  210-213.  doi: 10.13218/j.cnki.csdc.2015.04.007 摘要 ( 308 )   PDF(878KB) ( 302 )   以对甲基苯甲酰氯和甲苯为原料,无水AlCl3为催化剂,经过Friedel-Crafts酰基化反应得到4,4′-二甲基二苯甲酮(4,4′-DMBP)。再以4,4′-DMBP为原料,Aliquat 336 (甲基三辛基氯化铵)为相转移催化剂(PTC),通过KMnO4氧化合成了4,4′-二羧基二苯甲酮。同时采用红外光谱、核磁共振氢谱/碳谱以及高效液相色谱,对合成产品进行了表征分析。主要考察了PTC的催化活性、催化剂用量、反应温度、KMnO4用量和水的用量对反应体系的影响。实验表明,在中性条件下,当n(KMnO4)∶n(4,4′-DMBP)=8.5∶1,m(4,4′-DMBP)∶m(水)=3∶200,Aliquat 336用量为4,4′-DMBP物质的量的10%,反应温度为95 ℃时,产物的纯收率可达85.84%。 4,4′-Dimethylbenzophenone (4,4′-DMBP) was synthesized with p-toluoyl chloride and toluene as starting materials and anhydrous AlCl3 as catalyst through Friedel-Crafts acylation reaction.Then the 4,4′-DMBP was further oxidized by potassium permanganate in the presence of phase transfer catalyst (PTC) Aliquat 336 (trioctylmethylammonium chloride) and 4,4′-dicarboxylbenzophenone was synthesized as product.The product was characterized by HPLC,FTIR,1HNMR and 13CNMR.Effects of different factors,such as the activity of separate PTC,dosage of PTC,reaction temperature,dosage of potassium permanganate and water on the reaction yield were investigated.Results indicated that under neutral conditions,in the water at 95 ℃ by keeping the mole ratio of potassium permanganate to 4,4′-DMBP as 8.5∶1;the mass ratio of 4,4′-DMBP to water as 3∶200;dosage of Aliquat 336 as 10% (mole ratio) of 4,4′-DMBP,the reaction yield of the product achieves 85.84%. 参考文献 | 相关文章 | 计量指标

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无防腐剂护肤化妆品体系的防腐效能及安全性评价 Preservative efficacy and safety evaluation of antiseptic-free skin care cosmetics 刘文娟, 常志英 2015 (4):  214-217.  doi: 10.13218/j.cnki.csdc.2015.04.008 摘要 ( 505 )   PDF(813KB) ( 847 )   通过与传统防腐剂LGP的性能比较,分别考察了馨二醇68T+馨三醇复配体系和益生菌的防腐能力及安全性。结果表明:馨二醇68T+馨三醇复配体系对混合细菌的抑制能力优于混合真菌;益生菌对混合细菌和混合真菌的抑制能力基本相当;馨二醇68T+馨三醇复配体系和益生菌的抑菌能力均低于LGP;在防腐挑战试验进行到第7天时,2种无防腐剂日霜及精华液体系混合细菌和真菌的菌种量均小于10 cfu/g;3种精华液体系对人体的刺激性从高到低依次为:LGP>馨二醇68T+馨三醇>益生菌。 Preservative efficacy and safety property of SymDiol 68T+SymTriol and probiotics Leucidal Liquid SF were examined separately and compared with performance of the traditional antiseptics LGP.Results showed that inhibitive power of the blend system with SymDiol 68T+SymTriol against mixed bacteria is better than that of mixed fungi.Inhibitive power of natural antiseptics probiotics against mixed bacteria and against fungi is basically equivalent.Inhibitive power of both blend system SymDiol 68T+SymTriol and probiotics are lower than that of LGP.On the 7th day of preservative efficacy challenge test,amount of both mixed bacteria and mixed fungi in two kinds of day cream and essence liquid without antiseptics are less than 10 cfu/g.The irritation to skin of the three kinds of essence liquid decreases in the order of:LGP>SymDiol 68T+SymTriol>probiotics Leucidal Liquid SF. 参考文献 | 相关文章 | 计量指标

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白蜡树精苷的抗紫外线研究 Study on ultraviolet irradiation resistance effect of mandshurin 陈玉娟, 李成玉, 王巍, 钟子涛 2015 (4):  218-220.  doi: 10.13218/j.cnki.csdc.2015.04.009 摘要 ( 383 )   PDF(797KB) ( 322 )   通过培养人皮肤成纤维细胞(HSF)和采用人体法测定白蜡树精苷防晒霜的抗紫外线性能,研究了白蜡树精苷对HSF紫外线损伤的保护作用和白蜡树精苷防晒霜的防晒性能。结果表明,与正常培养的HSF相比,紫外线照射明显抑制了HSF的生长,而加入白蜡树精苷后,HSF在相同紫外线照射下生长明显优于不加白蜡树精苷的情况;通过人体法测试得到的白蜡树精苷防晒霜的SPF值为16,说明白蜡树精苷防晒霜有抗紫外线的作用,有望将白蜡树精苷添加到化妆品中,开发出能抵抗中等强度阳光紫外线照射的护肤品。 Protection action of mandshurin with respect to human skin fibroblastic strain (HSF) caused by ultraviolet irradiation as well as sunscreening performance of its formulated product was investigated via volunteers' body test method.Results showed that,as compared with the control group that is cultivated under conventional way,under same other conditions,the ultraviolet irradiation suppresses the growth of HSF significantly,while the addition of mandshurin improves the growth of HSF apparently.Via volunteers' body tests,the sun protection factor (SPF) of mandshurin sunscreening cosmetic cream was measured as 16 in-vivo.Obviously mandshurin sunscreening cosmetic cream displays good ultraviolet resistance action conspicuously.Hopefully,mandshurin might be added into cosmetics as sunscreening agent to resist ultraviolet irradiation of moderate sunshining. 参考文献 | 相关文章 | 计量指标

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红外光谱法在防晒化妆品鉴别研究中的应用 Application of Fourier transform attenuated total reflection infrared spectrometry in the identification of sunscreening cosmetics 孙婷, 穆同娜, 于晓瑾, 杨红梅, 赵丽, 吴燕涛 2015 (4):  221-225.  doi: 10.13218/j.cnki.csdc.2015.04.010 摘要 ( 285 )   PDF(942KB) ( 398 )   采用傅里叶变换衰减全反射红外光谱法(ATR-FTIR)对从不同渠道采集的6个同一品牌和系列的防晒化妆品进行分析,同时采用高效液相色谱仪对防晒化妆品样品中的防晒剂种类及其含量进行检测。结果表明,不同来源防晒化妆品样品的红外光谱图在防晒剂主要官能团结构上呈现较大差异,且与经高效液相色谱检测的防晒剂种类及含量结果具有较好的相关性。 Samples of six sunscreening cosmetic product of same brand and series but collected from separate distribution channels were analyzed with Fourier transform attenuated total reflection infrared spectrometry (ATR-FTIR).At the same time the variety and content of sunscreening agent in the cosmetic products were detected by high performance liquid chromatography (HPLC).Results showed that,in the FTIR spectra,there are quite big differences among the structure of main functional group of the sunscreening agent in the cosmetic product of same brand and series but collected from separate distribution channels.Further,the differences are quite conspicuously correlated with the variety and content of the sunscreening agent in the cosmetics detected by HPLC. 参考文献 | 相关文章 | 计量指标

专论与综述

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炮制技术在化妆品植物原料开发中的应用 Application of processing technique in developing plant materials in formulation of cosmetic products 邓小锋, 孟宏, 李丽, 刘有停, 董银卯 2015 (4):  226-229.  doi: 10.13218/j.cnki.csdc.2015.04.011 摘要 ( 318 )   PDF(922KB) ( 441 )   简要介绍了炮制方法,重点综述了植物通过炮制技术富集抗衰老、美白、抗敏等功效物质而实现增效的目的;最后总结了化妆品植物原料开发前景及存在的问题,为炮制技术在化妆品植物原料中的应用提供科学依据。 Methods used in processing technique of Chinese traditional herb medicine were briefed.Processing technique used for enrichment of substances with functional actions such as anti-senility,whitening,anti-allergy et al.in plant materials for purpose of efficacy upgrading were emphatically described.Prospects and existing problems in developing plant materials for cosmetic uses were summarized finally,which offers scientific bases for applying processing technique in using plant materials for cosmetic formulation. 参考文献 | 相关文章 | 计量指标

分析与检测

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离子色谱法测定氧化胺中的亚硝酸盐和硝酸盐 Determination of nitrate salts and nitrite salts in amine oxides by ion chromatography 刘振华, 张涌 2015 (4):  230-232.  doi: 10.13218/j.cnki.csdc.2015.04.012 摘要 ( 275 )   PDF(796KB) ( 321 )   建立了测定氧化胺中亚硝酸盐和硝酸盐的离子色谱分析方法。样品使用IC-C18反相吸附柱和0.45 μm的微孔水系滤膜处理后,经4.0 mmol/L Na2CO3和1.2 mmol/L NaHCO3混合淋洗液载入高性能阴离子专用色谱分析柱,并通过抑制型电导检测器检测。结果表明:NO2-和NO3-在质量浓度0.1~10.0 mg/L内线性关系良好,相关系数R2＞0.999 9;检出限分别为0.035和0.028 mg/L;相对标准偏差(RSD,n=7)为0.46%~2.24%;回收率为94.3%~102.5%。该方法具有简便、快速、准确、高效的特点,灵敏度高,安全实用,满足工业分析的要求。 A method for the simultaneous determination of nitrate salts and nitrite salts in amine oxides by ion chromatography was established.The amine oxide sample was pre-treated with IC-C18 reverse phase adsorption column and 0.45 μm micro-pore filter membrane,and then loaded into a high-performance anion exchange column with a mixed solution composed of 4.0 mmol/L Na2CO3 and 1.2 mmol/L NaHCO3 as eluant and detected with a suppressed conductivity detector.Results showed that good linear relationship displays within the range of nitrate and nitrite mass concentration between 0.1-10.0 mg/L with correlation coefficients (R2) more than 0.999 9.The detection limits of nitrate and nitrite were identified as 0.035 and 0.028 mg/L respectively.The relative standard deviations (RSD,n=7) lie 0.46%-2.24%.The spiked recoveries lie 94.3%-102.5%.This method has the features of simple,rapid,accurate and efficient.It is a high sensitive,safe and practical method,can meet the requirements of technical analysis. 参考文献 | 相关文章 | 计量指标

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离子排斥色谱法测定化妆品中硼酸(盐)含量 Determination of boric acid salt in cosmetics by ion exclusion chromatography 李铭, 凌小芳, 郑洪国, 郭桦 2015 (4):  233-240.  doi: 10.13218/j.cnki.csdc.2015.04.013 摘要 ( 306 )   PDF(815KB) ( 368 )   建立了离子排斥色谱法对化妆品中硼酸及硼酸盐类进行检测。在对试样进行前处理后,采用ICS1100离子色谱仪对硼酸及其盐类进行测定,配置对硼酸根具有良好选择性的IonPac ICE-borate离子排斥色谱柱为分析柱,以甲磺酸-甘露醇为淋洗液,利用抑制电导检测器对化妆品中硼酸盐进行检测。结果表明,硼酸盐的检出限为0.57 mg/kg,定量下限为1.9 mg/kg,回收率在87%~108%之间,具有良好的回收率和重现性。 The method of ion exclusion chromatography to detect boric acid and salt in cosmetics was established.After pretreatment of the samples,the boric acid and salt in samples was separated on ICS1100 ion chromatography system using IonPac ICE-borate ion exclusion column which has a good selectivity for borate radicals as analysis column,with methane sulfonic acid-mannitol as eluent,and suppressed conductivity detector to detect boric acid salts in cosmetics.Results showed that boric acid salt detection limit of this method is 0.57 mg/kg;the limit of quantification is 1.9 mg/kg;the recovery is in the range of 87%-108%,with good recovery and reproducibility. 参考文献 | 相关文章 | 计量指标