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2017年, 第47卷, 第8期　刊出日期：2017-08-22 上一期    下一期

基础研究

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双子表面活性剂N,N′-双十二烷基对苯二甲胺丙酸的合成及性能研究 Synthesis and performance of Gemini surfactant N,N′-bis(dodecyl)-1,4-xylylene diamine propionate acid 赵林秀, 李刚森, 王萍, 沈亚梅 2017 (8):  421-424.  doi: 10.13218/j.cnki.csdc.2017.08.001 摘要 ( 266 )   PDF(786KB) ( 370 )   以十二胺、丙烯酸甲酯和对二氯苄为原料,三氯甲烷为溶剂,合成了双子表面活性剂N,N′-双十二烷基对苯二甲胺丙酸。采用1H NMR和13C NMR对其结构进行了表征。(25±1) ℃时pH对产物表面活性的影响研究结果表明:pH分别为8,10和12时,cmc分别为1.6×10-5,3.3×10-5和2.1×10-5 mol/L;γcmc分别为32.39,33.24和36.94 mN/m;pc20分别为2.56,2.14和2.09;Γmax分别为3.45×10-6,3.97×10-6和4.34×10-6 mol/m2;Amin分别为0.48,0.42和0.38 nm2。当pH=12时,随溶液温度升高,pc20和Amin增大,Γmax减小。 Gemini surfactant N,N′-bis(dodecyl)-1,4-xylylene diamine propionate acid was synthesized from dodecylamine,methyl acrylate and p-xylylene dichloride as starting materials with trichloromethane as solvent.The chemical structure of the product was characterized by 1H NMR and 13C NMR.Performance of the product at (25±1) ℃ were studied and the results show that when the pH value is separately prepared at 8,10 and 12,the critical micellar concentration (cmc) is 1.6×10-5,3.3×10-5 and 2.1×10-5 mol/L respectively;the surface tension (γcmc) is 32.39,33.24 and 36.94 mN/m;the pc20 is 2.56,2.14 and 2.09;the Γmax is 3.45×10-6,3.97×10-6 and 4.34×10-6 mol/m2;the Amin is 0.48,0.42 and 0.38 nm2.When the pH value rises to 12,following the raise of temperature,the values of pc20 and Amin increase but the Γmax decreases. 参考文献 | 相关文章 | 计量指标

科技讲座

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离子液体表面活性剂的合成与应用(Ⅷ)——在分析中的应用 Synthesis and application of ionic liquid surfactants (Ⅷ) Application of ionic liquid surfactants in analysis 邹文苑, 杨许召, 王萍, 徐清杰, 王军 2017 (8):  425-429.  doi: 10.13218/j.cnki.csdc.2017.08.002 摘要 ( 269 )   PDF(1275KB) ( 347 )   离子液体表面活性剂同时具有有机溶剂的属性和优良的表面活性,在分析中得到了广泛应用。在微波/超声波辅助下,利用离子液体表面活性剂水溶液的胶束增溶作用,可对各种固体中的有机物进行萃取,同时也可以在萃取结束后加入化学试剂使水溶性表面活性剂变成水不溶性表面活性剂,实现原位预浓缩提高分析的灵敏度。离子液体表面活性剂可以作为HPLC的固定相、胶束动电毛细管色谱的准固定相等实现有机物的分离和手性拆分。离子液体表面活性剂通过与金属离子形成络合物实现增敏光谱测定金属离子。离子液体表面活性剂修饰电极后能够促进电子传递和提高电分析灵敏度。 Because of the dual properties of organic solvent and excellent surface activity,ionic liquid surfactants are widely used in analysis.Organics in solid material can be extracted with the micelle solubilization of ionic liquid surfactants under assistance of microwave/ultrasonic wave.Meanwhile,after completion of the extraction,chemical agents can be added to change the water soluble surfactant to water insoluble surfactant;so that the aqueous solution can be pre-concentrated in situ in order to better the sensitivity of the analysis.Ionic liquid surfactants can be used as stationary phase to separate organic compounds in HPLC or pseudo-stationary phase to enantioseparate chiral compounds in micellar electro kinetic chromatography.The sensitizing effect of ionic liquid surfactant media on the determination of metal ions is the result of complexing action of ionic liquid surfactant and metal ion.The electrode modified by ionic liquid surfactant can promote electron transfer and enhance sensitivity in electrochemical analysis. 参考文献 | 相关文章 | 计量指标

开发与应用

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双季铵盐改性纳米SiO2的乳化性能研究 Studies on the emulsifying performance of nano-SiO2 particles modified with bis-quaternary ammonium salts 黄威华, 邹华, 赖璐, 梅平 2017 (8):  430-434.  doi: 10.13218/j.cnki.csdc.2017.08.003 摘要 ( 239 )   PDF(7503KB) ( 84 )   用双季铵盐BQAS-16对纳米SiO2进行表面改性,并以改性后的纳米SiO2为乳化剂,制备了Pickering乳液。探究了改性比例、pH、盐的加入和油水体积比对Pickering乳液稳定性的影响。结果表明,与纳米SiO2相比,BQAS-16改性后的纳米SiO2具有更优异的乳化性能。随着BQAS-16用量的增加,乳液的稳定性增加。随着pH的增大,乳液的稳定性基本不变;但当pH增至13时,乳液的稳定性显著降低。随着NaCl浓度的增加,乳液的稳定性基本不变。当油水体积比为1∶1 时,乳液的稳定性最好。 Bis-quaternary ammonium salts BQAS-16 were used for the surface modification of nano-SiO2 particles,and the modified SiO2 nanoparticles were used as emulsifying agent for preparation of Pickering emulsion.Effects of the ratio of modification,the pH value,the addition of salt and the volume ratio of oil to water on the stability of Pickering emulsion were examined.Results show that the nano-SiO2 particles modified by BQAS-16 display better emulsifying performance as comparing with the nano-SiO2 particles.The stability of emulsion increases with increasing of the dosage of BQAS-16.With increasing the pH value,the stability of emulsion is basically no change.However,at the pH=13,the stability of emulsion decreases significantly.Moreover,as the NaCl dosage increases,the stability of emulsion is basically no change.When the volume ratio of oil to water is 1∶1,the emulsion is at the most stable state. 参考文献 | 相关文章 | 计量指标

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乳状液提高驱油效率的实验研究 Experimental study on emulsion enhancing displacement efficiency 祝仰文 2017 (8):  435-439.  doi: 10.13218/j.cnki.csdc.2017.08.004 摘要 ( 270 )   PDF(724KB) ( 370 )   通过柱状岩心模型,实验研究了乳状液的微观驱油特性。乳状液在不同渗透率岩心中的驱替实验结果显示,乳状液提高驱油效率的幅度与渗透率有关,乳状液的粒径范围与岩心孔径范围越接近,其驱油效率越高;乳状液中液滴对提高驱油效率发挥主要作用,而乳化剂对驱油效率的贡献相对很小。对于中高渗透率岩心,黏度相同的聚合物溶液与乳状液提高驱油效率值相近。 By columnar core model,the microscopic displacement characteristics of emulsion was studied.Experimental results of emulsion flooding in different permeability cores show that how well emulsion improve displacement efficiency is related to the permeability,and emulsion particle size range is closer to pore diameter range,the higher the displacement efficiency.Droplets in emulsion play a great role in enhancing displacement efficiency,while the contribution of emulsifiers in enhancing displacement efficiency is relatively small.For intermediate permeability cores,the displacement efficiency of polymer solution and emulsion with the same viscosity is similar. 参考文献 | 相关文章 | 计量指标

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铂负载AlPO-5催化剂的制备及其甘油催化氧化性能研究 Preparation of platinum-loaded AlPO-5 catalyst and its catalytic performance for glycerol oxidation 王超, 刘雷, 董晋湘 2017 (8):  440-445.  doi: 10.13218/j.cnki.csdc.2017.08.005 摘要 ( 309 )   PDF(2613KB) ( 315 )   采用水热合成法制备磷酸铝分子筛AlPO-5,并通过焙烧处理得到AlPO-5分子筛多孔材料,以浸渍法和沉淀法分别制备了Pt负载型AlPO-5催化剂,通过粉末XRD、TEM、氮气吸附-脱附等手段对制备的催化剂进行了对比表征,研究了负载方法对Pt团簇分散度以及粒径尺寸的影响。以Pt/AlPO-5作为催化剂,研究了其对甘油的催化氧化性能,系统考察了Pt负载量、还原方法和反应时间对甘油转化率和产物选择性的影响。实验结果表明,由浸渍法制备的催化剂对甘油的转化率和甘油醛的选择性较高,甘油醛的选择性最高可达到63.46%。甘油醛作为起始反应产物,其高选择性与较大尺寸的Pt纳米团簇有关。 Aluminum phosphate molecular sieve AlPO-5 was synthesized by hydrothermal method,and then calcined to obtain the porous AlPO-5 supporting material.Pt-loaded AlPO-5 catalyst was prepared by impregnation method and precipitation method,separately,and the catalyst was characterized by powder XRD,TEM and nitrogen adsorption-desorption.Effects of loading method on the dispersion of Pt clusters and particle size were examined;meanwhile,the catalytic performance of Pt/AlPO-5 on glycerol oxidation was studied.Effects of Pt loading,reduction method and reaction time on glycerol conversion and product selectivity were examined in detail.Results show that the catalyst prepared by impregnation method displays a higher conversion and selectivity of glyceraldehyde (up to 63.46%).Glyceraldehyde as a starting reaction product during glycerol oxidation,its high selectivity is closely related to Pt nanoclusters with larger size. 参考文献 | 相关文章 | 计量指标

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酶解羊胎盘抗氧化肽的分离及在护肤品中的应用 Separation of antioxidative peptides from sheep placenta byproduct by enzymolysis and its application in cosmetics 李明, 姜惠敏, 曹光群, 杨成 2017 (8):  446-451.  doi: 10.13218/j.cnki.csdc.2017.08.006 摘要 ( 396 )   PDF(831KB) ( 461 )   为开发酶解法制备的羊胎盘抗氧化肽在化妆品中的应用,采用木瓜蛋白酶酶解羊胎盘下脚料,通过DA201-C型大孔吸附树脂、超滤膜和Sephadex G-10葡聚糖凝胶色谱分离纯化,并对各组分进行抗氧化活性的测定,筛选得到具有较高DPPH自由基清除率的羊胎盘抗氧化肽S12。配制不同S12质量分数的护肤乳液和润肤晚霜,采用MC750型皮肤测试仪评价样品的保湿和弹性功效。结果表明,15名志愿者持续使用添加质量分数4% S12的护肤乳液和润肤晚霜60 d 后,角质层含水量分别增长了27和31,皮肤水分流失量分别降低了12.0和13.2 g/(m2·h),皮肤弹性参数R2分别升高了38%和45%。研究表明,添加了羊胎盘抗氧化肽的护肤品具有良好的保湿和提高皮肤弹性的功效。 In order to develop application of antioxidative peptides from sheep placenta byproduct by enzymolysis in cosmetics,papain was employed for the enzymolysis and DPPH radical scavenging activity of the hydrolysate was used for efficacy evaluation.The hydrolysate by papain was purified sequentially by DA201-C macroporous resin,ultrafiltration and Sephadex G-10 gel filtration.Fractions obtained from purification operations were evaluated.The sheep placenta peptide S12 displays the highest DPPH radical scavenging activity and was selected for further study.The formulas of skin care lotion and cream containing different content of S12 (0-5%) were designed,and the moisturizing and elastic effect of all skin care product samples were evaluated by MC750 skin test instrument.Results show that after continuous using the skin care lotion and cream containing 4% content of S12 for 60 d,the skin cuticula hydration of 15 volunteers increases by 27 and 31 respectively;the transepidermal water loss reduces by 12.0 and 13.2 g/(m2·h) respectively;and the skin elasticity R2 increases by 38% and 45% respectively.It is concluded that the skin care lotion and cream containing sheep placenta peptide can improve skin moisturizing and increase skin elasticity. 参考文献 | 相关文章 | 计量指标

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ZnO溶胶的制备及其抑菌性和光催化性能研究 Preparation of ZnO sol and its performance for bacteriostasis and photocatalytic degradation of organics 宋俊达, 陈洪龄 2017 (8):  452-457.  doi: 10.13218/j.cnki.csdc.2017.08.007 摘要 ( 377 )   PDF(1431KB) ( 337 )   以二水合醋酸锌和KOH为原料,聚乙烯吡咯烷酮(PVP)为表面修饰剂,制备了稳定透明的ZnO溶胶。利用X射线衍射仪、扫描电子显微镜、紫外可见分光光度计、荧光光谱仪和高效液相色谱仪对其进行了表征和测试。考察了二水合醋酸锌、KOH和PVP的用量对ZnO粒径及溶胶稳定性的影响;以金黄色葡萄球菌、大肠杆菌、绿脓杆菌、洋葱假单胞菌、白色念珠菌和黑曲霉为测试对象,采用琼脂稀释法测定ZnO溶胶的最小抑菌浓度(MIC);并对亚甲基蓝、乐果和乙酰甲胺磷溶液进行光催化性能研究。实验结果表明:在添加10 mmol二水合醋酸锌、15 mmol KOH和1.6 g PVP的较佳条件下合成的ZnO溶胶最为稳定,ZnO粒径分布均匀;ZnO溶胶有效地抑制了菌种的生长,其对金黄色葡萄球菌和洋葱假单胞菌的抑菌效果最好;同时高效地降解了亚甲基蓝、乐果和乙酰甲胺磷溶液,表现出较好的光催化活性。 Stabilized and transparent ZnO sol was prepared with zinc acetate dihydrate (ZAD) and potassium hydroxide (KOH) as starting materials and polyvinyl pyrrolidone (PVP) as surface modifying agent.The product was characterized and tested by X-ray diffraction,scanning electron microscopy,UV-visible absorption spectroscopy,fluorescence spectroscopy and high performance liquid chromatography.The influences of ZAD,KOH and PVP dosage on ZnO particle size and sol stability were examined.The minimum inhibitory concentration (MIC) value of ZnO sol were determined by agar dilution method with Staphylococcus aureus,Escherichia coli,Agrobacterium tumefaciens,Pseudomonas cepacia,Candida albicans and Aspergillus niger as testing objects.The photocatalytic activity of ZnO sol on degradation of methylene blue (MB),dimethoate and acephate solution was carried out.Results show that the ZnO sol product prepared with the stoichiometric composition of 10 mmol of ZAD,15 mmol of KOH and 1.6 g of PVP displays stable and uniformly distributed ZnO nanoparticle size.The growth of bacteria is inhibited effectively by the ZnO sol product,which has the best antibacterial effect on Staphylococcus aureus and Pseudomonas cepacia.Meanwhile,the ZnO sol product displays good photocatalytic activity on degradation of MB,dimethoate and acephate solution. 参考文献 | 相关文章 | 计量指标

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羟丙基-β-环糊精对化学防晒剂的包埋技术研究 Technology for encapsulation of chemical sun-screening agent with hydroxypropyl-β-cyclodextrin 邬凤娟, 张晨, 巴伊斯玛, 鲁旺旺, 甘亮, 曹光群 2017 (8):  458-462.  doi: 10.13218/j.cnki.csdc.2017.08.008 摘要 ( 393 )   PDF(717KB) ( 490 )   分别制备丁基甲氧基二苯甲酰基甲烷(BMDBM)和甲氧基肉桂酸乙基己酯(OMC) 2种化学防晒剂的羟丙基-β-环糊精包埋物,比较了超声法、研磨法和溶液搅拌法3种制备方法对化学防晒剂包埋率的影响,并利用正交试验优化包埋物的制备工艺。结果表明,溶液搅拌法最适用于2种化学防晒剂包埋物的制备,采用正交试验所得的较优工艺,BMDBM 和OMC的平均包埋率分别可以达到63.06%±2.5%和56.43%±2.0%。将2种化学防晒剂包埋物复配应用于防晒霜中,防晒剂包埋物具有良好的光稳定性。 Encapsulation compounds of butyl-methoxydibenzoylmethane (BMDBM) and octyl methoxycirmamate (OMC) were prepared separately by encapsulating with hydroxypropyl-β-cyclodextrin.Three encapsulation methods,including ultrasonic method,grinding method and solution stirring method were compared based on encapsulation ratio results.The preparation technology of encapsulation compounds was improved with orthogonal test.Results show that,solution stirring method is the most suitable method to prepare the encapsulation compounds.The encapsulation ratio of BMDBM and OMC in encapsulation compounds can be optimized by orthogonal test,and improved to 63.06%±2.5% and 56.43%±2.0% respectively.Encapsulation compounds can be applied in sun-screening cream,and display good photo-stability. 参考文献 | 相关文章 | 计量指标

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香叶天竺葵精油和纯露的挥发性成分分析及抗氧化活性评价 Analysis of volatile components and antioxidation activity evaluation of essential oil and aqueous extract from Pelargonium graveolens L′Herit. 任洪涛, 周斌 2017 (8):  463-467.  doi: 10.13218/j.cnki.csdc.2017.08.009 摘要 ( 489 )   PDF(709KB) ( 405 )   分别采用水蒸气蒸馏和同时蒸馏萃取法对香叶天竺葵精油和纯露的挥发性成分进行提取,通过气相色谱-质谱联用技术结合保留指数分析鉴定其化学组成,用峰面积归一化法确定各成分的相对含量。结果表明,香叶天竺葵精油中鉴定出71种化合物,主要成分有香茅醇、甲酸香茅酯、香叶醇、异薄荷酮、β-古芸烯、芳樟醇和惕各酸苯乙酯等;香叶天竺葵纯露中鉴定出39种化合物,主要成分有香茅醇、芳樟醇、香叶醇、异薄荷酮、α-松油醇、顺式芳樟醇氧化物和反式芳樟醇氧化物等。其中香叶天竺葵纯露中的挥发性成分大多存在于香叶天竺葵精油中,但含量存在较大的差异。采用 DPPH自由基和羟基自由基清除试验对香叶天竺葵精油和纯露的抗氧化活性进行评价。结果表明,香叶天竺葵精油和纯露均对DPPH自由基和羟基自由基具有一定的清除作用,香叶天竺葵纯露对DPPH自由基和羟基自由基的清除能力稍强于香叶天竺葵精油。 Volatile components of essential oil and aqueous extract from Pelargonium graveolens L′Herit. were prepared separately by steam distillation (SD) method and simultaneous distillation-extraction (SDE) method.Their compositions and relative contents were identified by gas chromatography-mass spectrometry (GC-MS) with retention index (RI) and peak area normalization method.Results show that a total of 71 volatile compounds are identified from the geranium essential oil,the main constituents being citronellol,citronellyl formate,geraniol,isomenthone,β-gurjunene,linalool and phenylethyl tiglate.A total of 39 volatile compounds are identified from the geranium aqueous extract,the main constituents being citronellol,linalool,geraniol,isomenthone,α-terpineol,cis-linalool oxide and trans-linalool oxide.The vast majority of volatile components in geranium aqueous extract exists in geranium essential oil,but their content is obviously different.Antioxidation activity of the essential oil and the aqueous extract were evaluated with 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical and hydroxyl radical scavenging methods.The experimental results show that both the geranium essential oil and the geranium aqueous extract display certain DPPH and hydroxyl radical scavenging activities.The DPPH and hydroxyl radical scavenging activity of geranium aqueous extract is higher than that of geranium essential oil. 参考文献 | 相关文章 | 计量指标

专论与综述

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两性双子表面活性剂合成研究进展 Progress in field for synthesis of zwitterionic Gemini surfactants 牟洪亮, 丁伟, 刘向斌, 王玲, 李振东, 程双 2017 (8):  468-475.  doi: 10.13218/j.cnki.csdc.2017.08.010 摘要 ( 330 )   PDF(884KB) ( 365 )   基于亲水基结构的不同,以阴-阳离子型、阴-非离子型和阳-非离子型进行分类对近年来出现的两性Gemini表面活性剂进行了介绍。重点综述了阴-阳离子型两性Gemini表面活性剂的合成,并简述了其性能及主要应用领域。最后提出了两性Gemini表面活性剂目前研究存在的不足,并对其未来研发的重点进行了展望。 Based on the different structure of the hydrophilic group,zwitterionic Gemini surfactants are currently classified as anionic-cationic,anionic-nonionic and cationic-nonionic.The synthesis process of anionic-cationic Gemini surfactants was emphatically summarized,and its properties and main application fields were briefly introduced.Finally,the shortcomings of study on zwitterionic Gemini surfactants were put forward and the future development of zwitterionic Gemini surfactants were prospected. 参考文献 | 相关文章 | 计量指标

分析与检测

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超高效液相色谱-质谱联用法同时测定化妆品中5种禁用性激素 Simultaneous determination of five banned sex hormones in cosmetics with UPLC-MS/MS 岳磊, 李晓静 2017 (8):  476-480.  doi: 10.13218/j.cnki.csdc.2017.08.011 摘要 ( 240 )   PDF(1002KB) ( 385 )   建立了同时测定化妆品中5种禁用性激素的超高效液相色谱-串联质谱法(UPLC-MS/MS)。采用ACQUITY UPLC®BEN C18色谱柱(2.1 mm×50 mm,1.7 μm),流动相为V(甲醇)∶V(0.1%的甲酸水溶液)=60∶40的混合溶液,流速0.4 mL/min,柱温30 ℃,进样量1 μL,扫描方式为多反应监测(MRM)联合相关信息扫描(IDA)与增强离子扫描(EPI)。结果表明,4种雌激素(雌二醇、雌三醇、雌酮和己烯雌酚)及黄体酮的线性范围为1~100 mg/L,方法的线性关系良好,相关系数均大于0.999。样品的平均回收率为79.8%~115.3%,RSD为1.43%~11.36% (n=6)。 A method using ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established for determination of five banned sex hormones in cosmetics.The chromatography column is selected as ACQUITY UPLC® BEN C18 column (2.1 mm×50 mm,1.7 μm).The mobile phase consists of methanol-0.1% formic acid aqueous solution (60∶40) and the flow rate is 0.4 mL/min.The column temperature is 30 ℃.Sample injection amount is 1 μL.The scanning method is multiple reaction monitoring (MRM) in combination with information dependent acquisition (IDA) and enhanced ion scanning (EPI).Results show that the relation between peak area and mass concentration of the detected four kinds of estrogen,including oestradiol,oestriol,oestrone and stilbestrol as well as progesterone displays good linearity with correlation coefficient higher than 0.999.Detection limit of the method is 1-100 mg/L.The method was carried out at three spiking levels,the average recoveries are in the range of 79.8%-115.3%,with relative standard deviations of 1.43%-11.36% (n=6). 参考文献 | 相关文章 | 计量指标