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    2014年, 第44卷, 第5期 刊出日期:2014-05-22 上一期    下一期
    基础研究
    海藻酸衍生物活化二氧化硅纳米粒制备Pickering乳液
    Preparation of Pickering emulsions with SiO2 nanoparticles activated with alginate derivative
    程春风, 李嘉诚, 颜慧琼, 刘若林, 王春修, 林强
    2014 (5):  241-246.  doi: 10.13218/j.cnki.csdc.2014.05.054
    摘要 ( 273 )   PDF(1646KB) ( 374 )  
    采用辛胺改性海藻酸钠,并以其通过物理混合和化学接枝2种途径活化SiO2纳米粒,利用红外光谱、核磁共振氢谱和动态光散射等对产物进行了表征,并超声乳化制备了其相应的Pickering乳液,进而对乳液的形貌进行了观察。结果表明:海藻酸钠上成功接枝了辛胺侧链;经2种途径活化后的SiO2纳米粒粒径均大于未活化的SiO2纳米粒,分别增至467.0和414.4 nm;其Zeta电位较SiO2纳米粒自身的-17.0 mV也发生了变化,分别为-43.9和-35.2 mV。同时,活化后的纳米粒具有了较好的乳化性能,尤其是通过表面化学接枝改性海藻酸钠的SiO2纳米粒,其形成的Pickering乳液液滴分散性好,大小均一,平均粒径为5 μm。 SiO2 nanoparticles were activated by octylamine modified sodium alginate via two ways,physical mixing and chemical grafting.The activated SiO2 nanoparticles were characterized by FTIR,1HNMR and DLS,et al.Then Pickering emulsions were prepared with the activated SiO2 nanoparticles under assistance of ultrasonic wave,and morphology of the emulsions was observed.Experimental results showed that octylamine side chain was successfully grafted onto the sodium alginate.The particle size of activated SiO2 nanoparticles via both physical mixing and chemical grafting ways is larger than that of unactivated SiO2 nanoparticles,and increases to 467.0 and 414.4 nm respectively.Surface potential of activated SiO2 nanoparticles changes to -43.9 and -35.2 mV respectively,which is lower than that of unactivated SiO2 nanoparticles,which shows a surface potential of -17.0 mV.Meanwhile,the activated SiO2 nanoparticles reveal better emulsifying properties,especially the nanoparticles activated by chemical grafting way could produce a more stable Pickering emulsion with better droplet dispersion,uniform size and with average particle diameter of 5 μm.
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    N,N′-双(月桂酰基)乙二胺二丙酸钠的复配性能研究
    Study on performances of sodium N,N′-bis(lauricethylenediamine)di-propionate
    吴崇珍, 包新颜, 许虎君
    2014 (5):  247-251.  doi: 10.13218/j.cnki.csdc.2014.05.055
    摘要 ( 235 )   PDF(848KB) ( 397 )  
    测定了N,N′-双(月桂酰基)乙二胺二丙酸钠(DLMC)及与十二烷基三甲基溴化铵(DTAB)和十二烷基聚氧乙烯(6)醚(AEO6)复配体系的表面张力,计算了DLMC及复配体系的表面化学性能参数;应用正规溶液理论得到复配体系内表面相和胶束相中2种表面活性剂之间的相互作用参数。结果表明,在25 ℃,0.1 mol·L-1 NaBr水溶液中,DLMC的临界胶束浓度(cmc)为1.01×10-4 mol·L-1,cmc下的表面张力(γcmc)为30.3 mN·m-1;DLMC/DTAB复配体系的γcmc,cmc和Amin均比单一组分要低;DLMC/AEO6复配体系的γcmc,cmc和Amin随着DLMC组分的增加先减小后有所增加。复配体系在形成胶束能力、降低表面张力效率及降低表面张力能力方面存在协同增效作用。 Surface tensions of sodium N,N′-bis(lauricethylenediamine) di-propionate (DLMC),DLMC/DTAB blend system and DLMC/AEO6 blend system were determined.The surface chemical parameters of DLMC as well as the blend systems were calculated.Interaction parameters between the two kinds surfactant in surface phase as well as micelle phase of the blend surfactant systems was calculated based upon normal solution theory.Results showed that in NaBr solution with concentration of 0.1 mol·L-1 under 25 ℃,cmc of DLMC is 1.01×10-4 mol·L-1,and γcmc is 30.3 mN·m-1.The γcmc,cmc and Amin of DLMC/DTAB blend system all are smaller than that of the single surfactant component in the blend system.The γcmc,cmc and Amin of DLMC/AEO6 blend system decrease at first,and then increase with the further addition of DLMC.The two blend systems exhibit synergic effect in both surface tension reduction capacity and efficiency,as well as capacity for formation of mixed micelles.
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    科技讲座
    表面活性剂的性能与应用(Ⅴ)——脂质体及其应用
    Performance and applications of surfactants (Ⅴ) Liposome and its applications
    苏鹏权, 赵莉, 徐宝财, 周雅文
    2014 (5):  252-256.  doi: 10.13218/j.cnki.csdc.2014.05.056
    摘要 ( 381 )   PDF(789KB) ( 596 )  
    首先简要介绍了脂质体的概念,总结了脂质体的常用制备方法,然后概述了脂质体的载药特性和靶向原理,列出了几种新型脂质体,最后重点综述了脂质体作为药物载体进行靶向给药的应用实例。 The concept of liposome was introduced briefly,and then the preparation methods were summarized.The characteristics of drug carrying and principles of targeting were described,followed by several novel kinds of liposome.Finally,the applications in targeted drug delivery were summarized.
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    开发与应用
    阳离子苯乙烯-丙烯酸酯微乳液表面施胶剂的制备
    Preparation of styrene-acrylate cationic microemulsion surface sizing agent
    李珩, 徐朝华
    2014 (5):  257-260.  doi: 10.13218/j.cnki.csdc.2014.05.057
    摘要 ( 282 )   PDF(1106KB) ( 584 )  
    以十六烷基三甲基溴化铵(CTAB)为乳化剂,正戊醇为助乳化剂,甲基丙烯酰氧乙基三甲基氯化铵(DMC)为阳离子单体,偶氮二异丙基咪唑啉盐酸盐(V-44)为引发剂,单体St/MMA/BA/MAA/DMC质量比为3.4/21.3/28.4/35.5/11.4,转速控制在180~230 r·min-1,反应温度控制在70~75 ℃时,得到阳离子苯乙烯-丙烯酸酯(以下简称为苯丙)微乳液,并利用红外光谱仪和差示扫描量热仪对微乳液进行了表征;粒径分析测得平均粒径为48 nm。将制得的苯丙微乳液用于纸张表面施胶后,纸张抗水性Cobb (30 s)值为16.5,抗张强度和表面强度比纸张施胶前分别增加约35.0%和40.6%。 Adopting cetyltrimethylammonium bromide as surfactant,n-pentanol as auxiliary emulsifier,methacryloxyethyltrimethylammonium chloride (DMC) as cationic monomer,2,2′-azobis[2-(2-imidazolin-2-yl)propane] dihydrochloride as initiator,with mass ratio of the reactants of styrene/methyl methacrylate/butyl acrylate/methacrylic acid/DMC monomer of 3.4/21.3/28.4/35.5/11.4;under agitation speed of 180-230 r·min-1 and polymerization temperature of 70-75 ℃,the cationic styrene-acrylate microemulsion was prepared.The product was characterized by FTIR and differential scanning calorimeter.Average particle size was measured as 48 nm.Application test of the prepared styrene-acrylate microemulsion on surface sizing of paper showed that the water resistance Cobb (30 s) value achieves 16.5,and tensile strength and surface strength of the paper increases 35.0% and 40.6% respectively as compared with that before the sizing.
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    一种聚硅氧烷消泡剂的合成与应用研究
    Preparation and application of polysiloxane defoamer
    王敏, 郭睿, 刘龙伟, 王二蒙, 解传梅, 宋艳艳
    2014 (5):  261-265.  doi: 10.13218/j.cnki.csdc.2014.05.058
    摘要 ( 306 )   PDF(968KB) ( 576 )  
    以氯铂酸为催化剂,烯丙醇聚氧乙烯聚氧丙烯醚(FB)、甲基丙烯酸十二烷基酯(LMA)和含氢硅油(PHMS)为原料,制得一种共改性硅油(PMS)。通过正交试验得到优化工艺条件为:n(Si-H)∶n(C=C)=1∶1.20,催化剂用量30 μg·g-1,反应温度90 ℃,反应时间6 h,此条件下转化率达93.45%。采用高速剪切乳化搅拌方式将水相在油相中进行乳化,制备出聚硅氧烷消泡剂,由应用测试得到优化配方为:硅膏质量分数10%,PMS质量分数6%,复合乳化剂(m(Span 60)∶m(Tween 60)∶m(OP-10)=3∶2∶1)质量分数4%,制备出的聚硅氧烷消泡剂稳定性好,其消抑泡性能优于市售同类产品。 A kind of modified silicone oil (PMS) was synthesized by hydrosilylation with allyl alcohol polyethoxy polypropoxy ether (FB),lauryl methacrylate (LMA) and hydrosilicone oil (PHMS) as starting materials,as well as chloroplatinic acid as catalyst.Optimum reaction conditions were investigated via orthogonal designed experiments as:molar ratio,n(Si-H)∶n(C=C)=1∶1.20;dosage of catalyst,30 μg·g-1;reaction temperature,90 ℃ for 6 h.Under these conditions,the conversion achieves 93.45%.The polysiloxane defoamer was prepared by emulsifying of aqueous phase into the oil phase,which was composed of silicone oil paste,blended emulsifying agent and the prepared PMS in a high speed shearing emulsification mixer.The optimized formulation was obtained via application tests as:mass fraction of silicone oil paste,10%;mass fraction of PMS,6%;and mass fraction of blended emulsifying agent (composed of Span 60,Tween 60 and OP-10 with mass ratio of 3∶2∶1), 4%.The polysiloxane defoamer product shows good stability and its defoaming property and foam inhibition property is superior to other similar products.
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    掺羟基磷灰石牙膏对早期龋的修复及吸附镉离子作用研究
    Effect of toothpaste containing hydroxyapatite on restoration of early stage caries and cadmium ion adsorption
    马伟群, 黄建生, 徐平平
    2014 (5):  266-269.  doi: 10.13218/j.cnki.csdc.2014.05.059
    摘要 ( 312 )   PDF(976KB) ( 409 )  
    通过掺羟基磷灰石(HA)牙膏对早期龋模型进行处理,应用扫描电镜和显微硬度计对再矿化效果进行分析,同时将掺HA牙膏和空白牙膏分别配成不同质量浓度的牙膏悬液,分别加入0.2 mg·L-1的镉离子溶液中,静置24 h后去上清液用电感藕合等离子发射光谱仪测定残余镉离子的量,比较2种牙膏对水溶液中镉离子的吸附情况。结果显示,处理1和2周时掺HA牙膏组釉质的显微硬度分别为253.87±5.66和291.90±10.37,而空白牙膏组则分别仅为199.73±7.11和200.07±9.84,有统计学意义(P<0.05);扫描电镜下可见HA处理对早期龋脱矿牙釉质再矿化作用明显;各质量浓度组的掺HA牙膏对镉离子的吸附率均高于空白牙膏。结果表明将HA掺入牙膏可提高其修复早期龋的作用,同时增强了对水中镉离子的吸附作用。 Models of tooth with early stage caries were treated with suspension of toothpaste containing hydroxyapatite (HA).The effect of re-mineralization of tooth enamel surface was assessed by scanning electron microscopy and microhardness value measurement.Cadmium ion solutions with initial mass concentration of 0.2 mg·L-1 were mixed with toothpaste suspensions with and without addition of HA respectively and then been kept still for 24 h.The residual cadmium ion mass concentration of the supernatant was measured by inductively coupled plasma emission spectrometer and the adsorption effect of cadmium ion was calculated.Results showed that the toothpaste containing HA could significantly re-mineralize and improve the microhardness of artificial enamel caries.The Vicker's hardness values were 253.87±5.66 and 291.90±10.37 in HA group,higher than that of 199.73±7.11 and 200.07±9.84 in control group (P<0.05).The adsorption rate of cadmium ion of toothpaste containing HA is higher than that of the control group.
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    云母钛珠光颜料在洗发水体系中悬浮稳定性的研究
    Study of suspension stability of mica titanium dioxide pearl pigment in hair shampoo system
    陈小康, 徐卡秋, 马红鹏, 卢二凯, 张真
    2014 (5):  270-272.  doi: 10.13218/j.cnki.csdc.2014.05.060
    摘要 ( 606 )   PDF(791KB) ( 457 )  
    为了提高云母钛珠光颜料在洗发水体系中的悬浮稳定性,采用5种表面改性剂对云母钛珠光颜料进行表面改性。实验结果表明,云母钛珠光颜料经正十八醇表面改性后其在基础洗发水体系中的悬浮分散稳定性得到有效改善。在适宜的改性条件下,改性后云母钛珠光颜料在基础洗发水体系中的初始沉降时间由改性前的0.2 h延长到2.2 h,完全沉降时间由6.0 h延长到46.5 h。 In order to improve the suspension stability of mica titanium dioxide pearl pigment in hair shampoo system,five kinds of surface modifiers were used for the surface modification of mica titanium dioxide pearl pigment.Experimental results showed that octadecanol can effectively improve the suspension stability of mica titanium dioxide pearl pigment in hair shampoo base.In appropriate modification conditions,the initial settling time increased from 0.2 to 2.2 h,fully settling time increased from 6.0 to 46.5 h.
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    复合广谱紫外线吸收剂在防晒化妆品中的应用研究
    Application of composite UV absorbent in sun-screening cosmetics
    陈庆生, 孟潇, 龚盛昭, 孔胜仲, 孙永
    2014 (5):  273-277.  doi: 10.13218/j.cnki.csdc.2014.05.061
    摘要 ( 302 )   PDF(793KB) ( 450 )  
    采用紫外分光光度法对16种中草药提取液的紫外线吸收效果进行筛选和复配研究。结果表明,由罗勒、草果、款冬花、山姜、椴树花、鼠尾草和槐米等中草药的提取液等质量组成的组合物具有较佳紫外线吸收效果,并与化学紫外线吸收剂进行了组合优化,优化组合(质量分数)为:甲氧基肉桂酸乙基己酯7.0%、奥克立林2.0%、二乙氨羟苯甲酰基苯甲酸己酯3.0%。当天然紫外线吸收剂组合物为5.0%,与优化的化学紫外线吸收剂组合物复配,应用产品的SPF值可达31.1,PFA值为8.7,达到了广谱紫外线吸收的效果,应用产品的刺激性也大大降低。 Ultraviolet spectrophotometry for selecting and compounding of 16 kinds of natural UV absorbents was studied.Results showed that a blend composed of extract of equal mass of Chinese traditional herb medicines namely,Basil,Tsaoko,Coltsfoot flower,Alpinia,Linden tree flower,Sage and Sophora japonica displays good UV protection effect.Meanwhile,chemical UV absorbents were also studied to find an optimized UV absorbing formulation.Combination and amount of chemical UV absorbents were optimized as follows:ethylhexyl methoxycinnamate,7.0%;octocrylene,2.0%;diethylamine hydroxybenzoyl hexyl benzoate,3.0%.The application research was done,and results showed that when 5% of the UV absorbent blend made of Chinese traditional herb medicines is compounded with the optimized blend made of chemical UV absorbent combination,the SPF and PFA value of application product achieves 31.1 and 8.7 respectively,which meets the required effect of protection from broad-spectrum UV and the skin irritation of the product reduces significantly.
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    救必应提取物安全性研究
    Study on safety of extract of Ovateleaf Holly Bark
    徐春生, 徐文霞
    2014 (5):  278-281.  doi: 10.13218/j.cnki.csdc.2014.05.062
    摘要 ( 435 )   PDF(805KB) ( 346 )  
    通过急性毒性试验、亚慢性毒性试验、沙门氏菌/回复突变试验、细胞微核试验、口腔黏膜影响试验和牙龈黏膜影响试验等,对救必应提取物在牙膏中使用的安全性进行了评价。结果表明,救必应提取物属于实际无毒级物质,无基因突变和染色体畸变的危险,对口腔黏膜和牙龈黏膜无刺激,可安全应用于牙膏等口腔护理产品之中。 For evaluating the safety of the extract of Ovateleaf Holly Bark that adopted in toothpaste,the acute toxicity test,sub-chronic toxicity test,salmonella typhimurium/reverse mutation assay,mammalian erythrocyte micronucleus test,oral mucosa impact test and gingival mucosa impact test were conducted.Test results showed that the extract of Ovateleaf Holly Bark belongs to practically non-toxic grade material,and there is no danger of gene mutation and chromosome aberration,no stimulation to mouth mucosa and gingiva.So it can be safely applied to oral care product.
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    2-苄基乙酰基乙酸乙酯的催化合成研究
    Catalytic synthesis of ethyl 2-benzylacetoacetate
    王树清, 王歆然, 高崇
    2014 (5):  282-284.  doi: 10.13218/j.cnki.csdc.2014.05.063
    摘要 ( 245 )   PDF(748KB) ( 378 )  
    以乙酰乙酸乙酯、氯化苄和氢氧化钾为原料,在相转移催化剂的作用下合成了2-苄基乙酰基乙酸乙酯。考察了反应时间、反应温度、催化剂类型和用量以及投料比等对产品收率的影响。结果表明,优化工艺条件为:以四丁基溴化铵为催化剂,水为溶剂,n(乙酰乙酸乙酯)∶n(氯化苄)∶n(氢氧化钾)∶n(水)∶n(四丁基溴化铵)=1∶1.15∶1.2∶7.4∶0.012,反应温度100 ℃,反应时间5 h,此条件下产品收率达90.54%。 Ethyl 2-benzylacetoacetate was synthesized with ethyl acetoacetate,benzyl chloride and potassium hydroxide as starting materials and tetrabutylammonium bromide as phase transfer catalyst.Effects of reaction time,reaction temperature,catalyst dosage and the molar ratio of the reactants were examined.Results showed that under the optimized reaction conditions as:mole ratio,n(ethyl acetoacetate)∶n(benzyl chloride)∶n(KOH)∶n(H2O)∶n(tetrabutylammonium bromide)=1∶1.15∶1.2∶7.4∶0.012;reaction temperature,100 ℃ for 5 h;yield of the product reaches 90.54%.
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    专论与综述
    Bola型表面活性剂研究新进展
    Recent progress in research work with respect to bolaform surfactants
    陈鹏, 郑成, 毛桃嫣, 张利萍
    2014 (5):  285-291.  doi: 10.13218/j.cnki.csdc.2014.05.064
    摘要 ( 309 )   PDF(2061KB) ( 485 )  
    介绍了Bola型表面活性剂的合成以及应用,展示了其独特的结构和性质。阐述了阳离子型、阴离子型、两性型和非离子型等Bola型表面活性剂的具体合成方法,并对其在构建离子通道、基因转染、纳米材料合成等应用方面进行了归纳,最后对其在当今工业领域的应用进行展望。 Synthesis and applications of bolaform surfactants were presented,with their unique structure and performance demonstrated.Detailed methods for preparation of cationic,anionic,zwitterionic and nonionic bolaform surfactants were described.Meanwhile,their uses in the construction of ion channel,gene transfection,and preparation of nano materials and so on were summarized.Their future applications in the industrial fields were prospected.
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    分析与检测
    含氢硅油和聚醚硅油中含氢量的测定
    Determination of hydrogen content in hydrogen containing silicon oil and polyether silicon oil
    李春静, 田莉瑛, 吕静, 齐广辉, 李琰, 柳文庆
    2014 (5):  292-294.  doi: 10.13218/j.cnki.csdc.2014.05.065
    摘要 ( 773 )   PDF(815KB) ( 507 )  
    采用龙氏氮素器对含氢硅油和聚醚硅油中的含氢量进行了测定。其原理是利用Si-H键与NaOH溶液反应产生氢气,通过准确测定生成氢气的体积,由气态方程式即可计算出含氢量,并与化学法进行了对比,结果表明两者间相对偏差均小于3.3%,取得了满意的效果。 The determination of hydrogen content in hydrogen containing silicon oil and polyether silicon oil was conducted with Lunge apparatus,which is originally designed for determination of nitrogen content in organic materials.Its principle is based on the reaction between NaOH and Si-H bond with generation of hydrogen gas and the volume of the hydrogen gas is accurately measured.Then the hydrogen content can be determined via gas equation calculation.The results were compared with that obtained from chemical analysis method and showed that the relative deviation is less than 3.3%,which denotes that the method is satisfactory in practice.
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    凝胶渗透色谱-液相色谱-串联质谱法同时测定化妆品中15种糖皮质激素和性激素
    Simultaneous determination of 15 kinds of glucocorticoid and sex hormone in cosmetics by GPC-LC-MS/MS
    崔晗, 沈葆真, 陈溪, 曹文军, 刘梦遥, 黄大亮
    2014 (5):  295-298.  doi: 10.13218/j.cnki.csdc.2014.05.066
    摘要 ( 295 )   PDF(799KB) ( 304 )  
    建立了一种凝胶渗透色谱-液相色谱-串联质谱法同时测定化妆品中15种糖皮质激素和性激素的方法。化妆品样品采用乙腈超声提取,环己烷-乙酸乙酯体系的凝胶渗透色谱柱净化,以乙腈-体积分数为0.1%甲酸水溶液作为流动相,经C18色谱柱进行分离,由液相色谱-串联质谱仪定量检测。结果表明,方法的线性关系良好,相关系数R均大于0.995,方法检出限为0.1~4.0 mg·kg-1,添加平均回收率为70.0%~104.0%,相对标准偏差为5.3%~15.5%。 A method for the simultaneous determination of residue of 15 kinds of glucocorticoid and sex hormone in cosmetics by gel permeation chromatography-liquid chromatography-tandem mass spectrometry (GPC-LC-MS/MS) was established.The sample was extracted with acetonitrile under ultrasonic assistance,and the extract was purified with GPC column of cyclohexane-ethyl acetate.Then the contents in the purified extract were separated by a C18 column with acetonitrile-0.1% formic acid solution as the mobile phase,and then detected by LC-MS/MS.Testing results showed that good linearity was obtained with correlation coefficients higher than 0.995.The detection limit ranges within 0.1-4.0 mg·kg-1.The spiked recovery ranges within 70.0%-104.0%,and the RSD ranges within 5.3%-15.5%.
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