当期目录

2014年, 第44卷, 第2期　刊出日期：2014-02-22 上一期    下一期

基础研究

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两亲性聚(甲基丙烯酸甲酯-co-甲基丙烯酸)胶束包覆维生素A Encapsulation of vitamin A with amphiphilic poly(methyl methacrylate-co-methacrylic acid) micelles 卓小露, 倪鑫炯, 徐晓进, 曹玉华, 曹光群, 邢小平 2014 (2):  61-65.  doi: 10.13218/j.cnki.csdc.2014.02.014 摘要 ( 279 )   PDF(2863KB) ( 377 )   采用透析法制备了包覆维生素A的两亲性聚(甲基丙烯酸甲酯-co-甲基丙烯酸)[P(MMA-co-MAA)]胶束。对空白、载药聚合物胶束的粒径、Zeta电位、形貌进行了比较;考察维生素A加入量对包覆率和载药量的影响;考察包覆前后维生素A的贮藏稳定性;并对维生素A包覆胶束模拟缓释进行了研究。结果表明:数均摩尔质量为64 886 g·mol-1、单体摩尔比为7∶3的双亲性无规聚合物P(MMA-co-MAA)在0.1 mol·L-1硼砂缓冲液(pH=9.2)中的临界胶束浓度(cmc)为0.050 g·L-1;包覆维生素A的胶束粒径比空白胶束增大近1倍,Zeta电位变得更负;当维生素A加入量为包覆材料的15%时,包封率和载药量分别达到81.9%和13.5%;包覆后的维生素A在光照60 d后保留率仍能达到56.3%,而维生素A在自然光照下的半衰期仅为15 d,有效延长了维生素A的贮存时间;载药胶束在接近皮肤表面pH的磷酸盐缓冲液(pH=5.0)中10 h内稳定释放76.1%的维生素A,可应用于化妆品中。 Amphiphilic polymer poly(methyl methacrylate-co-methacrylic acid) [P(MMA-co-MAA)] micelles were applied to encapsulate vitamin A with dialysis method.The loaded micelles were compared with blank micelles in respect of particle size,Zeta potential and morphology.Effect of amount of vitamin A on encapsulation degree and loading extent were investigated respectively.Storage stability of the vitamin A before and after encapsulation was investigated.Meanwhile,stimulated slow releasing action of encapsulated vitamin A was studied.Results showed that critical micelle concentration of random polymer P(MMA-co-MAA) with number-averaged mole mass of 64 886 g·mol-1 and monomer mole ratio 7∶3 in 0.1 mol·L-1 borax buffer solution (pH=9.2) is 0.050 g·L-1.Particle size of micelles of encapsulated vitamin A achieves nearly double of that of the blank micelles,and Zeta potential becomes more negative.When the amount of vitamin A added is 15% of the encapsulating material,the encapsulation degree and loading extent achieves 81.9% and 13.5% respectively.Under exposure of natural light,half life of vitamin A is only 15 d,while vitamin A encapsulated by P(MMA-co-MAA) micelles,still retains 56.3% after exposed to natural light for 60 d.It means that encapsulation of vitamin A with the P(MMA-co-MAA) can improve its storage stability effectively.The accumulative slow releasing of vitamin A by loaded micelles in the phosphate buffer solution (pH=5.0,which is similar to that of human skin) achieves 76.1% in 10 h.It shows that the vitamin A loaded micelles have good application prospect in cosmetics. 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(Ⅱ)——表面活性剂的反胶束及其应用 Performance and applications of surfactants (Ⅱ) Reversed micelles and their applications 赵秋瑾, 徐宝财, 赵莉, 张桂菊 2014 (2):  66-69.  doi: 10.13218/j.cnki.csdc.2014.02.015 摘要 ( 330 )   PDF(845KB) ( 456 )   简要介绍了反胶束的结构和基本性质,总结了较为常用的反胶束体系。重点综述了反胶束技术的应用进展,阐述了反胶束萃取技术及反胶束在制备纳米材料和酶促反应等方面的应用。最后提出了目前存在的问题并对其应用前景进行了展望。 Structure and properties of reversed micelles were introduced and the commonly used reversed micelle systems were summarized,with progress in research work refers to applications of reversed micelles focused.The reversed micellar extraction technology as well as the application of the technology in the field of preparing nano-materials and enzymatic catalysis reaction was expounded.Some existing problems were pointed out and the development outlooks were prospected. 参考文献 | 相关文章 | 计量指标

开发与应用

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随机质心衍射法优化合成1,1,1,3,5,5,5-七甲基三硅氧烷的工艺研究 Optimization of the process for synthesizing 1,1,1,3,5,5,5- heptamethyltrisiloxane by Random-Centroid Optimization Method 龚红升, 胡文斌, 廖列文, 张蔚欣, 王昶童 2014 (2):  70-74.  doi: 10.13218/j.cnki.csdc.2014.02.016 摘要 ( 261 )   PDF(825KB) ( 407 )   选用含氢量为1.4%的高含氢硅油(DH)和六甲基二硅氧烷(MM)为原料,强酸型离子交换树脂作催化剂,采用随机质心衍射优化法对1,1,1,3,5,5,5-七甲基三硅氧烷(MDHM)的合成工艺进行优化。此过程仅用了13次试验,优化所得工艺条件为:m(DH)∶m(MM)=1∶13.03,催化剂用量为6.34%,反应温度65.3 ℃,反应时间8.15 h,在该条件下所得产物的平均产率为39.56%。 Synthesis of 1,1,1,3,5,5,5-heptamethyltrisiloxane (MDHM) was processed by adopting high hydrogen-content silicone (DH) that containing 1.4% (mass fraction) of hydrogen and hexamethyldisiloxane (MM) as starting materials and strong acidic ion exchange resin as catalyst.The synthesis process was optimized by applying Random-Centroid Optimization Method.Only 13 tests were needed for the optimization and results showed that the optimal conditions were as follows:reaction mass ratio,m(DH)∶m(MM)=1∶13.03;dosage of the catalyst,6.34%;reaction temperature and time,65.3 ℃ and 8.15 h,respectively.Average yield of the product achieves 39.56%. 参考文献 | 相关文章 | 计量指标

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端氨丙基聚二甲基硅氧烷的合成研究 Synthesis of aminopropyl end capped polydimethylsiloxane 罗啸秋, 张利萍, 吴海龙, 雷秋芬 2014 (2):  75-78.  doi: 10.13218/j.cnki.csdc.2014.02.017 摘要 ( 421 )   PDF(819KB) ( 404 )   以1,3-双(3-氨基丙基)-1,1,3,3-四甲基二硅氧烷(氨丙基封端剂)和八甲基环四硅氧烷(D4)为原料,在四甲基氢氧化铵((CH3)4NOH)硅醇盐的催化下合成端氨丙基聚二甲基硅氧烷。较佳的反应条件为:反应温度80~90 ℃,反应时间5 h,催化剂硅醇盐用量(相对于D4的质量)0.75%。同时对封端剂的用量(Wf)与产物黏度(η25)、产物实际氨值(W′NH)的对应关系以及产物重均相对分子质量(Mw)与黏度的关系进行研究。通过红外光谱对产物结构进行分析,结果表明氨丙基封端剂成功参与反应。 With 1,3-Bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane (aminopropyl end capping agent) and octamethylcyclotetrasiloxane (D4) as starting materials,aminopropyl end capped polydimethylsiloxane was synthesized under the catalysis of tetramethylammonium hydroxide ((CH3)4NOH) silanolate.The optimum conditions were obtained as follows:reaction temperature 80-90 ℃;reaction time 5 h;dosage of silanolate catalyst 0.75% (based on total mass of D4).The relationship between the dosage of capping agent (Wf) and product viscosity (η25) as well as actual amine equivalence of the product (W′NH),and the relationship between the average molecular weight (Mw) and product viscosity were studied.Structure of the product was characterized by IR spectrum,and the result showed that the end capping agent reacted with D4 successfully. 参考文献 | 相关文章 | 计量指标

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水性油墨助剂十二胺基氯乙酸钠的合成与性能研究 Synthesis and properties of dodecylamine sodium chloroacetate as water-based printing ink additive 杨禄, 蒋平平, 张萍波, 高学文, 乔倩倩 2014 (2):  79-82.  doi: 10.13218/j.cnki.csdc.2014.02.018 摘要 ( 306 )   PDF(805KB) ( 483 )   以十二胺和二氯乙酸为原料合成十二胺基氯乙酸钠(DSC)。粗产品十二胺基氯乙酸(DCA)的较佳合成工艺条件为:n(二氯乙酸)∶n(十二胺)=1∶1.5,催化剂用量为1%,于120 ℃下反应18 h,产率为58.91%。对目标产物DSC采用IR进行结构表征,由表面活性分析可知其cmc为3.38×10-3 mol·L-1,γcmc为27.43 mN·m-1,通过吸光度及粒径分析得到对水溶性油墨色浆分散性较好时其用量为1.6%。 Dodecylamine sodium chloroacetate (DSC) was synthesized from dodecylamine and dichloroacetic acid as starting materials.The first step product is dodecylamine chloroacetic acid (DCA).Optimum reaction conditions for preparing DCA were determined as:mole ratio of dichloroacetic acid to dodecylamine 1∶1.5;mass fraction of the catalyst 1%;reaction time 18 h at 120 ℃.The DCA yield achieves 58.91%.Structure of the final product DSC was characterized by IR.The measurement results for surface activities of the final product showed that critical micelle concentration (cmc) of DSC achieves 3.38×10-3 mol·L-1 and lowest surface tension (γcmc) of DSC achieves 27.43 mN·m-1.The dispersing property of DSC was identified by UV-vis and ZetaPALS,and the optimum mass fraction of DSC as dispersant in water-based printing ink is 1.6%. 参考文献 | 相关文章 | 计量指标

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曝气法臭氧氧化处理高含量烷基多苷废水的研究 Study of aeration process for ozone treatment of waste water containing high content of alkyl polyglucosides 武明亮, 张涛革, 张文俊, 张晓文, 郭丽潇, 王旭东 2014 (2):  83-86.  doi: 10.13218/j.cnki.csdc.2014.02.019 摘要 ( 210 )   PDF(850KB) ( 424 )   通过研究曝气盘孔径对泡沫性能、泡沫量及有机质降解的影响,了解曝气法臭氧氧化处理高含量烷基多苷废水的规律。结果表明:随着曝气盘孔径的减小,产生的泡沫的粒径、发泡比逐渐减小,泡沫的持液量、泡沫半衰期逐渐增大;臭氧的通入量为28 g时,产生的泡沫总量、消耗单位臭氧降解的COD值、COD的降解率均随曝气盘孔径的减小而增大;采用孔径150和40 μm的曝气盘组合式处理工艺与单纯孔径150 μm的曝气盘处理工艺比较,COD降解率提高了6.8百分点,每克臭氧降解的COD值提高了54.5 mg,臭氧的利用率显著提高,而产生的泡沫总量较采用孔径80 μm的曝气盘减少了约2/3。 Aeration process for treatment of waste water containing high content of alkyl polyglucosides was investigated via study of effect of aeration diffuser disc aperture on foam performance,foam volume generated and organic matter degradation.Results showed that,following the reducing of the aeration diffuser disc aperture,bubble size of the foam and the foaming ratio gradually decreases;while the total liquid hold and half-life of the foam gradually increases.When the ozone introduced achieves 28 g,the total foam volume generated,the degradation level of COD of per gram ozone consumed and the degree of degradation of COD increases following the reducing of aeration diffuser disc aperture.Performance of combination of aeration diffuser discs with 150 and 40 μm apertures was compared with that of single 150 μm,the COD degradation of the former is 6.8 percent points higher than that of the latter,and COD degraded by one gram of ozone increases 54.5 mg.The utilization efficiency of ozone increases remarkably.Further,total foam volume generated by the combined aeration diffuser discs reduces by 2/3 as compared with that of single aeration diffuser disc with aperture of 80 μm. 参考文献 | 相关文章 | 计量指标

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一种橘皮精油干洗剂的研制 Preparation of a dry-cleaning agent with mandarin peel essential oil 胡生发, 花儿 2014 (2):  87-89.  doi: 10.13218/j.cnki.csdc.2014.02.020 摘要 ( 279 )   PDF(749KB) ( 565 )   以D-柠檬烯为干洗主体溶剂,制备了一种橘皮精油干洗剂。以去污效率为指标,考察了表面活性剂用量及配比、纯化水及乙醇的添加对去污效率的影响,并通过正交试验对各影响因素进行了优化。结果表明,干洗剂的优化配比(质量分数)为:表面活性剂(AES+AEO3)总量为2.0%,其中m(AES)∶m(AEO3)=1∶4,乙醇为5.0%,纯化水为0.3%,余量为D-柠檬烯。此优化条件下去污效率可达97.6%。 A dry-cleaning agent with mandarin peel essential oil in which D-limonene is the main effective component was prepared.Effect of composition and dosage of surfactant,as well as addition of purified water and ethanol on detergency of the prepared dry-cleaning agent was investigated via orthogonal designed experiments.Results showed that the optimized ratio (mass fraction) was identified as:dosage of surfactant,2% composed of AES and AEO3 with mass ratio m(AES)∶m(AEO3)=1∶4;dosage of ethanol 5.0%;dosage of water 0.3%;and the balance is D-limonene.Detergency of the product achieves 97.6%. 参考文献 | 相关文章 | 计量指标

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锆掺杂氧化锌复合紫外屏蔽材料的制备及表征 Preparation and characterization of composite UV-shielding material made of Zr doped zinc oxide 江琦, 唐泽晴 2014 (2):  90-93.  doi: 10.13218/j.cnki.csdc.2014.02.021 摘要 ( 229 )   PDF(2668KB) ( 390 )   以Zn(NO3)2,ZrOCl2和NaOH为主要原料,采用共沉淀-水热法制备了晶型规整的掺Zr纳米ZnO复合紫外屏蔽材料。研究了Zr的掺杂量、水热温度、水热时间和Zr的掺杂方式等对材料紫外屏蔽性能的影响,得到了制备掺Zr纳米ZnO紫外屏蔽材料较好的制备条件为:共沉淀掺杂,Zr掺杂量为3.5%,水热温度150 ℃,水热时间0.5 h。采用X射线衍射仪和透射电镜对样品进行了表征,结果表明,样品晶型好、尺寸均匀。 Zr doped zinc oxide composite UV-shielding material with regular crystal form was prepared by hydrothermal co-precipitation method with zinc nitrate,zirconium oxychloride and sodium hydroxide as starting materials.Effects of dosage of Zr doping material,temperature and time for hydrothermal treatment and method for Zr doping on the UV-shielding performance of the product were investigated.The optimum preparation conditions were identified as:dosage of doped Zr,3.5%;temperature and time of hydrothermal treatment,150 ℃ and 0.5 h respectively.The final product was characterized by X-ray diffraction (XRD) and transmission electron microscope (TEM).Results showed that the product displays good crystal form and uniform size. 参考文献 | 相关文章 | 计量指标

专论与综述

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对称型双子表面活性剂的合成研究进展 Progress in research work with respect to synthesis of symmetric gemini surfactants 侯宝峰, 王业飞, 刘宏刚, 王桂杰 2014 (2):  94-99.  doi: 10.13218/j.cnki.csdc.2014.02.022 摘要 ( 338 )   PDF(956KB) ( 452 )   简要介绍了对称型双子表面活性剂的合成原理,包括极性头基加入法、疏水链加入法和联接链加入法;详细综述了各种对称型双子表面活性剂按照不同原理的合成路线,包括阳离子型双子表面活性剂、阴离子型双子表面活性剂、非离子型双子表面活性剂、两性离子型双子表面活性剂、具有特殊结构和功能的双子表面活性剂及多聚体等;简单总结了各种合成路线的优缺点,并对对称型双子表面活性剂的发展趋势和应用前景进行了展望。 Principles for synthesis of symmetric gemini surfactants,including polar head group addition method,hydrophobic chain addition method and coupling chain addition method were briefed.Synthesis routes for various types of symmetric gemini surfactants including cationic gemini surfactants,anionic gemini surfactants,nonionic gemini surfactants,zwitterionic gemini surfactants,as well as gemini surfactants with special structures and functions and their polymers prepared in accordance with different principles were described in detail.A brief summary of the advantages and disadvantages of various synthesis routes was listed and development trends and application of symmetric gemini surfactants were prospected. 参考文献 | 相关文章 | 计量指标

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香料香精的安全性及防范措施与评价标准 Safety and safety guarding measures as well as safety evaluation criteria for flavors and fragrances 陈娟, 尹学琼 2014 (2):  100-104.  doi: 10.13218/j.cnki.csdc.2014.02.023 摘要 ( 399 )   PDF(812KB) ( 562 )   综述了香料香精的分类;主要介绍了天然香料的自源性安全性及其在种植、采摘、粗加工、提取以及包装和储藏过程中的安全性及其防范措施;并简单介绍了目前国际上致力于发展香料香精安全性的机构和组织,并对他们的主要贡献进行了介绍;同时,介绍了目前国内关于香料香精的安全评价标准;最后对香料香精安全性的健康发展进行了展望。 Classification of flavors and fragrances were summarized.Autogenous safety issues of natural flavors and fragrances as well as the safety issues,safety guarding measures in the processes for their planting,plucking,gathering,preliminary processing,extraction,packaging and storing were presented.The international institutions and organizations that engaged in safety issues of flavors and fragrances and their main contributions were introduced.Meanwhile,the safety evaluation criteria currently applied in China were described.Outlooks for development of safety guarding measures in this field were prospected. 参考文献 | 相关文章 | 计量指标

分析与检测

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人参香皂中人参总皂苷含量的测定 Determination of total ginsenoside content in ginseng-formulated toilet soap 曲正义, 刘宏群, 赵景辉, 姚春林, 王英平 2014 (2):  105-107.  doi: 10.13218/j.cnki.csdc.2014.02.24 摘要 ( 300 )   PDF(761KB) ( 350 )   采用超声提取法对人参香皂中的人参总皂苷进行提取,溶剂萃取法对人参总皂苷进行纯化,用香草醛-高氯酸比色法对纯化后样品进行了人参总皂苷含量的测定,检测波长为540 nm。实验结果表明,香草醛-高氯酸比色法在0.02~0.24 mg内线性关系良好(r=0.999 5),平均回收率为96.04%,RSD为2.29% (n=5)。所测6种人参香皂中人参总皂苷的质量分数为1.72~9.66 mg·g-1。 Ginseng-formulated toilet soap sample was extracted by ethanol under assistance of ultrasonic action.Then the extract was purified by extraction with a series of solvents.Total ginsenoside content in the purified extract sample was determined by vanillin-perchloric acid colorimetry with detection wavelength of 540 nm.Results showed that the relationship between the absorbance and the ginsenoside content displays good linearity within range of 0.02-0.24 mg (r=0.999 5) and average recovery rate was 96.04% with a relative standard deviation of 2.29% (n=5).Determination test with samples of six kinds of ginseng-formulated toilet soap was carried out and the total ginsenoside content lies within 1.72-9.66 mg·g-1. 参考文献 | 相关文章 | 计量指标

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离子色谱法同时测定化妆品中氟离子、碘离子、溴酸根和氰根 Simultaneous determination of ions of fluoride,iodide,bromate radical and cyanide radical in cosmetics by ion chromatography 林立, 王海波, 李仁勇 2014 (2):  108-111.  doi: 10.13218/j.cnki.csdc.2014.02.025 摘要 ( 314 )   PDF(989KB) ( 333 )   采用离子色谱法同时测定化妆品中氟离子、碘离子、溴酸根和氰根。对化妆品样品的前处理方法和仪器条件进行了优化,以氢氧化钠溶液进行梯度淋洗,阴离子分析柱(IonPacAS11-HC,250 mm×4 mm)分离,氰根采用电化学检测器进行定量,氟离子、碘离子和溴酸根采用电导检测器进行定量。结果表明,氟离子、溴酸根、碘离子和氰根的检出限分别为2.0,10.0,10.0和1.0 mg·kg-1。各离子的回收率为78.5%～110.6%,相对标准偏差为1.9%～6.9%。对实际样品进行检测,满足化妆品中多离子的检测要求。 A method for simultaneous determination of ions of fluoride,iodide,bromate radical and cyanide radical in cosmetics by ion chromatography was established.Conditions for pre-treatment of samples of cosmetics as well as operation of the instrument were optimized.NaOH solution was used as gradient elution agent and the anions were separated by an analysis column (IonPacAS11-HC,250 mm×4 mm).Content of the cyanide radical ion was quantified by electrochemical detector,while the fluoride ion,iodide ion and bromate radical ion were quantified by conductivity detector.The detection limits of fluoride ion,bromate radical ion,iodide ion and cyanide radical ion are 2.0,10.0,10.0 and 1.0 mg·kg-1 respectively.The spiked recoveries are in the range of 78.5% to 110.6%.The relative standard deviations are 1.9% to 6.9%.The method can meet requirements of multiple ion detection in cosmetics. 参考文献 | 相关文章 | 计量指标

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反相高效液相色谱法测定化妆品中的神经酰胺 Determination of ceramides by reversed phase high performance liquid chromatography 缪晓琴, 金抒 2014 (2):  112-114.  doi: 10.13218/j.cnki.csdc.2014.02.026 摘要 ( 505 )   PDF(769KB) ( 508 )   采用反相高效液相色谱法测定化妆品中的神经酰胺。色谱条件为:SHIMADZU Shim-pack VP-C18ODS (150 mm×4.6 mm,5 μm)色谱柱,C18ODS保护柱芯,流动相V(甲醇)∶V(异丙醇)=55∶45,流速1.0 mL·min-1,柱温30 ℃,紫外检测器检测,波长205 nm,检测池温度40 ℃。结果表明,在此色谱条件下,神经酰胺在0～5 g·L-1与相应的峰面积具有良好的线性关系(r=0.991 4),线性回归方程为A=1 466 341ρ,回收率在96.5%～101.2%。 A reversed phase high performance liquid chromatography (RP-HPLC) method for the determination of ceramides in cosmetics was established.The sample was analyzed on a SHIMADZU Shim-pack VP-C18ODS (150 mm×4.6 mm,5 μm) with C18ODS guard column core and UV detector.Operating conditions were:mobile phase consisted of V(methanol)∶V(isopanol)=55∶45 at a flow rate of 1.0 mL·min-1;column temperature 30 ℃;wavelength of the UV detector 205 nm;detection cell temperature 40 ℃.Results showed that as the mass concentration of ceramide is in the range of 0-5 g·L-1,the relationship between mass concentration and the corresponding peak area shows good linearity (r=0.991 4).The regression equation can be expressed as A=1 466 341ρ and the recovery achieves 96.5%-101.2%. 参考文献 | 相关文章 | 计量指标

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化妆品中咪唑烷基脲的定量分析方法 Quantitative analysis of imidazolidinyl urea in cosmetics 汪敏, 金晶 2014 (2):  115-117.  doi: 10.13218/j.cnki.csdc.2014.02.027 摘要 ( 575 )   PDF(1102KB) ( 545 )   建立了一种基于测定咪唑烷基脲释放甲醛的量而对于化妆品中咪唑烷基脲的定量分析方法。咪唑烷基脲在Nash's试剂作用并在一定温度下释放甲醛,经分光光度法测定不同时间的甲醛释放量可用于咪唑烷基脲的定量分析。结果表明,60 ℃下水浴1 h可使咪唑烷基脲中甲醛释放量达到稳定,1 mol的咪唑烷基脲可释放1.116 mol的甲醛。咪唑烷基脲在化妆品中的最低检出限是0.2 mg·L-1,加标回收率为75%~98%。 A method for quantitative analysis of imidazolidinyl urea in cosmetics based upon determination of amount of formaldehyde released from imidazolidinyl urea was established.Formaldehyde was released by the action of Nash's reagent on imidazolidinyl urea under a certain constant temperature.Amount of formaldehyde released at different time was measured via spectrophotometric method and can be used for the quantitative analysis of imidazolidinyl urea.Results showed that,under 60 ℃ for 1 h,release of the formaldehyde from imidazolidinyl urea can achieve a stable state and completed.1 mol of imidazolidinyl urea can release 1.116 mol of formaldehyde.The lowest limit of detection is 0.2 mg·L-1 and the spiked recoveries of the method range within 75%-98%. 参考文献 | 相关文章 | 计量指标