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2014年, 第44卷, 第11期　刊出日期：2014-11-22 上一期    下一期

基础研究

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含十二烷基的聚甲基丙烯酸N,N-二甲氨基乙酯的合成及性能研究 Preparation and properties of poly[2-(N,N-dimethyl amino) ethyl methacrylate] with dodecyl group 周建华, 王海龙, 贺仁妍 2014 (11):  601-604.  doi: 10.13218/j.cnki.csdc.2014.11.134 摘要 ( 228 )   PDF(979KB) ( 374 )   以偶氮二异丁腈(AIBN)为引发剂、2-{[(十二烷基硫基)硫代甲酰基]硫烷基}琥珀酸(DCTSS)作为链转移剂、甲基丙烯酸N,N-二甲氨基乙酯作为单体,通过可逆加成-断裂链转移聚合法合成含十二烷基的聚甲基丙烯酸N,N-二甲氨基乙酯(PDMAEMA-C12H25)。探讨反应温度以及链转移剂与引发剂摩尔比对聚合的影响,采用核磁共振氢谱和凝胶渗透色谱对产物结构及相对分子质量进行表征,同时测试了聚合物的表面性能。结果表明,反应温度为70 ℃,链转移剂与引发剂摩尔比为4:1时,PDMAEMA-C12H25的相对分子质量分布较窄,反应可控,具有较低的临界胶束浓度(0.022 g·L-1),最低表面张力为33.8 mN·m-1 (25 ℃),对染料具有良好的分散作用。 Poly[2-(N,N-dimethyl amino) ethyl methacrylate] with dodecyl group (PDMAEMA-C12H25) was synthesized via the reversible addition-fragmentation chain transfer (RAFT) free radical polymerization with 2-{[(dodecy-sulfenyl)-carbonothionyl]sulfanyl} succinic acid (DCTSS) as chain transfer agent and AIBN as initiator.The effects of some parameters on the polymerization of DMAEMA were investigated,such as temperature,molar ratio of the chain transfer agent to the initiator.The structures and molecular weight of the products were characterized by 1HNMR and GPC.Meanwhile,surface properties of the product were measure.Results showed that at the reaction temperature of 70 ℃ and the molar ratio of the chain transfer agent to the initiator of 4:1,the molecular weight distribution of PDMAEMA-C12H25 is narrow and the reaction is controllable.The product displays rather lower critical micelle concentration (0.022 g·L-1) with lowest surface tension of 33.8 mN·m-1 (at 25 ℃),and good dispersing action for dyestuffs. 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(Ⅺ)——表面活性剂的泡沫作用及其应用 Performance and applications of surfactants (Ⅺ) Foaming action of surfactant and its applications 刘媛飞, 胡俊, 赵莉, 徐宝财, 韩富 2014 (11):  605-610.  doi: 10.13218/j.cnki.csdc.2014.11.135 摘要 ( 286 )   PDF(825KB) ( 582 )   首先介绍了泡沫的结构和性质,探讨了表面活性剂在泡沫的生成、稳定和破裂中的作用;叙述了表面活性剂的泡沫性能及其评价方法;最后综述了表面活性剂的泡沫性能在浮选分离、油田开发、消防等领域的应用,并对其发展前景进行了展望。 Structure and properties of foam were briefed.Actions of surfactant in formation,stabilization and breaking of foam were discussed.Foaming performance of surfactant and methods for its evaluation were described.Finally,applications of foaming performance of surfactant in fields of flotation separation,oil-field exploitation and fire extinguishment were summarized as well as its future development was prospected. 参考文献 | 相关文章 | 计量指标

开发与应用

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酯基三甲氧基有机硅季铵盐的合成及其表面活性 Synthesis and surface activity of the ester group trimethoxy organosilicon quaternary ammonium salt 陈瑞兰, 张俊杰, 毛桃嫣, 郑成 2014 (11):  611-614.  doi: 10.13218/j.cnki.csdc.2014.11.136 摘要 ( 244 )   PDF(795KB) ( 317 )   以硬脂酸、N,N-二甲基乙醇胺(DMEA)和γ-氯丙基三甲氧基硅烷为原料合成酯基三甲氧基有机硅季铵盐,采用FTIR,ESI-MS和1HNMR对中间体及终产物进行了结构表征,结果与目标结构一致。通过正交试验,得到中间体硬脂酸二甲基乙醇胺酯的优化合成工艺条件:反应温度为180 ℃,反应时间为8 h,n(硬脂酸):n(DMEA)=1:1.6,催化剂用量为原料总质量的0.5%。季铵化合成产物的优化工艺条件:在N2保护下,反应温度为110 ℃,n(硬脂酸二甲基乙醇胺酯):n(γ-氯丙基三甲氧基硅烷)=1:1.4,催化剂用量为原料总质量的0.5%,反应时间为28 h。并通过稳态荧光法测得产物在298 K下的临界胶束浓度为0.009 3 g·L-1。 An ester group trimethoxy organosilicon quaternary ammonium salt was synthesized with stearic acid,dimethylethanolamine (DMEA) and γ-chloropropyl trimethoxy siloxane as starting materials.Structure of the product was characterized by FTIR,ESI-MS and 1HNMR,and the characterization results showed that the product is accord with the target.Via orthogonal designed experiments,the optimum reaction conditions for preparing the intermediate stearic acid dimethylethanolamine ester were obtained as:reaction temperature,180 ℃;reaction time,8 h;mole ratio,n(stearic acid):n(DMEA)=1:1.6;dosage of the catalyst,0.5%;and for the quaternarization,reaction temperature,110 ℃ under nitrogen atmosphere;mole ratio,n(stearic acid dimethylethanolamine ester):n(γ-chloropropyl trimethoxy siloxane)=1:1.4;dosage of the catalyst,0.5%;reaction time,28 h.The cmc of the product under 298 K were determined by steady-state fluorescence analysis as 0.009 3 g·L-1. 参考文献 | 相关文章 | 计量指标

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羟乙基对苯二胺硫酸盐染发剂的制备及性能研究 Preparation and performance of hair dye based upon hydroxyethyl-p-phenylenediamine sulfate 岳娟, 高海燕, 徐宇, 陈秦君 2014 (11):  615-619.  doi: 10.13218/j.cnki.csdc.2014.11.137 摘要 ( 683 )   PDF(1235KB) ( 353 )   以羟乙基对苯二胺硫酸盐为染料中间体制备氧化型染发剂,并对染色工艺进行优化。在此基础上,对染后样品进行一系列性能检测,并与对苯二胺进行比较。结果表明,羟乙基对苯二胺硫酸盐具有较好的抗氧化能力,且当pH=9,40 ℃染色20 min时染色深度最大且对毛发损伤较小。与对苯二胺相比,羟乙基对苯二胺硫酸盐对毛发损伤更小,较好地保持了毛发结构的完整性,且染后的毛发具有较好的抗紫外性能。 Hydroxyethyl-p-phenylenediamine sulfate was used as dye intermediate to prepare hair dye.Meanwhile,the dyeing operating conditions were optimized.On this basis,a series of performance test for the dyed samples were conducted,and the results showed that,hydroxyethyl-p-phenylenediamine sulfate displays good oxidation resistance;and under conditions as pH 9,temperature 40 ℃ and time 20 min,the dye depth is biggest with comparatively less hair damage.At the same time,the results were compared with that of conventional hair dye based upon p-phenylenediamine,and it showed that the hair damage caused by hydroxyethyl-p-phenylenediamine sulfate is smaller and the hair retains good structural integrity under the same conditions.Furthermore,the dyed hair exhibits good UV-resistance. 参考文献 | 相关文章 | 计量指标

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一种美白乳液的制备与稳定性研究 Preparation and stability study of a lightening emulsion 舒鹏, 孔胜仲, 龚盛昭 2014 (11):  620-623.  doi: 10.13218/j.cnki.csdc.2014.11.138 摘要 ( 365 )   PDF(771KB) ( 517 )   通过对含美白剂十一碳烯酰基苯丙氨酸和苯乙基间苯二酚的乳化体系稳定性研究,探讨了配方中乳化剂种类与用量、油脂溶解能力、增稠体系选择、均质乳化参数控制等主要影响因素,得出了稳定美白乳液配方和工艺参数为:乳化剂采用质量分数为2.00%的PEG-20甲基葡糖倍半硬脂酸酯、质量分数为1.00%的甲基葡糖倍半硬脂酸酯和质量分数为0.30%的硬脂酰谷氨酸钠(质量分数为1.50%的鲸蜡醇磷酸酯钾);油脂选用质量分数为3.00%的甲氧基肉桂酸乙基己酯和质量分数为7.00%的辛基十二醇;增稠剂选用质量分数为2.00%的硬脂酸、质量分数为0.40%的丙烯酸羟乙酯/丙烯酰二甲基牛磺酸钠共聚物和质量分数为0.10%的黄原胶,乳化温度85 ℃,均质速度9 000 r·min-1。 Stability of an emulsion system composed of undecylenoyl phenylalanine and phenylethyl resorcinol was studied.Main factors that affect stability of the emulsion,such as kinds and dosage of the emulsifying agent,emulsifying agent solubility in oil,selection of the thickening agent system,control of the emulsification homogenizer operating parameters et al.were investigated.Then the formulation and operating conditions for the preparation of the stable emulsion were identified as follows:composition (mass fraction) of emulsifying agant,2.00% of PEG-20 methyl glucose sesquistearate,1.00% of methyl glucose sesquistearate and 0.30% of sodium stearoyl glutamate (1.50% of potassium cetyl alcohol phosphate);composition (mass fraction) of oil phase,3.00% of ethylhexyl methoxycinnamate and 7.00% of octyldodecanol;composition (mass fraction) of thickening agents,2.00% of stearic acid,0.40% of hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer and 0.10% of xanthan gum;emulsification temperature,85 ℃;homogenizer speed,9 000 r·min-1. 参考文献 | 相关文章 | 计量指标

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浊点萃取法提取黑种草子粕抗氧化剂的工艺研究 Cloud point extraction technology of antioxidizing components from Nigella glandulifera seed meal 刘学, 曹莹粲, 韩王康, 杨成, 曹光群 2014 (11):  624-627.  doi: 10.13218/j.cnki.csdc.2014.11.139 摘要 ( 214 )   PDF(786KB) ( 336 )   采用浊点萃取法提取黑种草子粕(NGSM)中抗氧化活性成分,以对DPPH自由基清除率为考察指标,采用单因素试验和正交试验考察在浊点萃取过程中各关键因素对清除率的影响,确定较佳提取条件为:表面活性剂质量浓度40 g·L-1,液固比35:1,离子强度0.513 mol·L-1,平衡时间50 min。提取物质量浓度为40 g·L-1时,对DPPH自由基的平均清除率为86.87%,且呈剂量效应关系。 Cloud point extraction (CPE) was applied for the extraction of antioxidizing components from Nigella glandulifera seed meal (NGSM).The extraction technology was optimized by single factor experiment and orthogonally designed experiment with scavenging ratio of free radical of 1,1-diphenyl-2-trinitro-phenyl hydrazine (DPPH) as indicator for antioxidizing activity of the extract.The optimum extraction conditions were obtained as follows:surfactant mass concentration,40 g·L-1;liquid-solid ratio,35:1;ion strength,0.513 mol·L-1;and equilibration time,50 min.Under such conditions,the average DPPH free radical scavenging ratio achieves 86.87%,and the efficacy is related to its dosage. 参考文献 | 相关文章 | 计量指标

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化妆品微生物检验影响因素的探讨 Study on affecting factors of microbiological inspection of cosmetics 谢小保, 杨秀茳, 孙廷丽, 李彩玲, 文霞 2014 (11):  628-630.  doi: 10.13218/j.cnki.csdc.2014.11.140 摘要 ( 301 )   PDF(1290KB) ( 365 )   通过设置加中和剂和不加中和剂2个实验组,按照《化妆品卫生规范》(2007年版)中规定的平板培养法对化妆品中微生物进行检验,对2组实验的菌落检测情况进行比较分析。结果显示:加入中和剂的实验组,化妆品稀释10倍可检出菌落;不加入中和剂的实验组,18种化妆品稀释100倍可检出菌落,2种膏霜类化妆品稀释1 000倍可检出菌落。表明中和剂能够减少检测时化妆品的稀释倍数;另外,氯化三苯基四氮唑(TTC)对化妆品中的细菌有抑制作用,TTC影响检测结果的准确性。建议在化妆品稀释液中添加中和剂,降低培养基中TTC浓度,在标准中增加方法验证试验,以70%回收率作为判定试验有效性的依据。 Via setting up of two experimental groups,in which one composed of neutralizing agent and another without it,microbial inspection was carried out according to plate culture method that specified in China Hygienic Standard for Cosmetics.Experimental results on the colony detection of the two groups were compared.In the group with neutrazing agent added,10-fold dilution of cosmetics can be detected colonies,while in the group without neutralizing agent added,100-fold dilution of 18 cosmetics can be detected colonies,and 1 000-fold dilution of 2 creams can be detected colonies.Such results showed that the neutralizing agent can reduce the dilution of cosmetics when detection.Further,it was also found that TTC (2,3,5-triphenyl terazolium chloride) can inhibit the growth of bacteria in the cosmetics,so that TTC will affect the accuracy of the test results.It is recommended that verification test should be incorporated in the test standard;neutralizing agent should be added in the diluted solution of the cosmetics to reduce concentration of TTC in the culture medium;and 70% recovery of the test bacteria should be taken as the criteria for determining validity of the test. 参考文献 | 相关文章 | 计量指标

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pH敏感魔芋葡甘聚糖复合凝胶的制备及其缓释性能研究 Preparation and controlled releasing behavior of pH-sensitive konjac glucomannan complex gel 许东颖, 王婴, 孟巨光, 林韶彬 2014 (11):  631-634.  doi: 10.13218/j.cnki.csdc.2014.11.141 摘要 ( 300 )   PDF(1315KB) ( 347 )   以魔芋葡甘聚糖(KGM)-黄原胶(XG)共混多糖为载体,进一步复配β-环糊精(β-CD)得到KGM/XG/β-CD复合干凝胶;以香兰素为模型香精,制备了装载香精的KGM/XG/β-CD复合凝胶,研究了装载香兰素的复合凝胶的释放行为,并与KGM/XG复合凝胶的释放行为做了比较。结果表明:在pH分别为5,7和9的缓冲液中,KGM/XG/β-CD复合凝胶中的香兰素12 h后累积释放率分别为29.5%,47.7%和60.6%,较KGM/XG复合凝胶中的香兰素在12 h后累积释放率(分别为45.0%,69.3和82.3%)低,表明具有空腔结构的β-CD对香兰素的释放起到了较好的缓释作用。 Mixed polysaccharide of konjac glucomannan (KGM) and xanthan gum (XG) was used as the carrier and then β-cyclodextrin (β-CD) was further blended with the carrier to obtain KGM/XG/β-CD complex dry gel.Then vanillin was used as model flavor to prepare flavor loaded complex gel.Controlled releasing behavior of the flavor loaded complex gel was investigated and the results were compared with that of KGM/XG complex gel.Results showed that in buffered solutions of separate pH of 5,7 and 9 and after 12 h,the cumulative content of vanillin released from the KGM/XG complex gel reaches 45.0%,69.3% and 82.3% respectively;while that from the KGM/XG/β-CD complex gel reaches 29.5%,47.7% and 60.6%,respectively,which are significantly lower.Such results indicated that the cavity structure of β-CD provides a controlled releasing effect on vanillin. 参考文献 | 相关文章 | 计量指标

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两步法合成王朝酮的工艺研究 Technology for two-step synthesis of aroma chemical dynascone 马洪亮, 李锐, 吴奇林, 姜兴涛 2014 (11):  635-637.  doi: 10.13218/j.cnki.csdc.2014.11.142 摘要 ( 427 )   PDF(746KB) ( 407 )   以脱氢芳樟醇为原料,先在多聚磷酸(PPA)的催化下进行重排,同时发生环化后得到1-乙酰基-5,5-二甲基-1-环己烯,然后再进行烷基化反应生成目标产物王朝酮,两步反应的总产率达40.8%。产物用IR,1HNMR,13CNMR和GC-MS等进行了表征。探讨了反应温度、催化剂用量及催化剂重复使用次数对中间体1-乙酰基-5,5-二甲基-1-环己烯产率的影响,结果表明:反应温度为80 ℃,脱氢芳樟醇与多聚磷酸的质量比为1:2条件下中间体产率较高,可达到97.0%,催化剂多聚磷酸可重复使用2~3次。 Firstly 1-acetyl-5,5-dimethyl-1-cyclohexene was obtained via rearrangement cyclization reaction with dehydrolinalool as starting material and poly-phosphoric acid (PPA) as catalyst,and then via the alkylation reaction to synthesize the targeted product dynascone.The overall yield of the two steps achieves 40.8%.The product was characterized by IR,1HNMR,13CNMR and GC-MS.Effect of dosage of the catalyst,reaction temperature and catalyst reusing on yield of 1-acetyl-5,5-dimethyl-1-cyclohexene was investigated.Results showed that yield of 1-acetyl-5,5-dimethyl-1-cyclohexene achieves 97.0% based on 80 ℃ of reaction temperature and mass ratio of dehydrolinalool to PPA 1:2.The catalyst PPA can be reused for 2~3 times. 参考文献 | 相关文章 | 计量指标

专论与综述

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碳氢/碳氟混杂型表面活性剂的研究进展 Progress in research work with respect to hydrocarbon/fluorocarbon hybrid surfactants 杨美, 郝京诚, 李洪光 2014 (11):  638-643.  doi: 10.13218/j.cnki.csdc.2014.11.143 摘要 ( 217 )   PDF(2800KB) ( 296 )   阐述了分子中同时含有一条碳氢链和一条碳氟链的碳氢/碳氟混杂型表面活性剂的基本概念,介绍了该类表面活性剂的发展历史、研究现状及典型分子的合成方法,归纳了其流变特性、聚集行为及其在乳化、生物医药等领域的实际应用,提出应从分子结构设计入手,有针对性地研发新一代碳氢/碳氟混杂型表面活性剂。 Basic conception for hydrocarbon/fluorocarbon hybrid surfactants where both a hydrocarbon chain and a fluorocarbon chain are integrated into the same surfactant molecule was introduced.Their development history,research work status and synthesis method for typical molecules were described.Their rheological characteristics,aggregation behavior and practical applications in fields of emulsification and biomedicine were summarized.It was put forward that the development of new generation of hydrocarbon/fluorocarbon hybrid surfactants should be orientatively proceeded from molecular structure design. 参考文献 | 相关文章 | 计量指标

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双子表面活性剂的合成及应用研究进展 Progress in field of research work with respect to synthesis and applications of Gemini surfactants 高南, 李国荣, 陈旭东 2014 (11):  644-651.  doi: 10.13218/j.cnki.csdc.2014.11.144 摘要 ( 511 )   PDF(947KB) ( 931 )   综述了近年来国内外双子(Gemini)表面活性剂的合成、性能及应用研究的进展。介绍了目前离子型、非离子型、两性离子型及不对称型Gemini表面活性剂的主要合成方法以及它们的主要性能;阐述了Gemini表面活性剂在日用化工、乳液聚合、金属防腐、生物技术和三次采油等各领域的应用状况。最后对Gemini表面活性剂的发展方向进行了展望。 The recent domestic and international progress in field of research and development work with respect to syntheses,properties and applications of functional Gemini surfactants were reviewed.Main synthesis methods and performances of ionic,nonionic,amphoteric and asymmetric Gemini surfactants were described.Applications of Gemini surfactants in daily use chemicals,emulsion polymerization,metal corrosion prevention,biotechnology and tertiary oil recovery were discussed as well.Furthermore,the prospective future of Gemini surfactants was also prognosticated. 参考文献 | 相关文章 | 计量指标

分析与检测

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固相萃取-液相色谱-串联质谱法测定祛痘化妆品中硝基咪唑类药物 Determination of nitroimidazoles in acne dispelling cosmetics with solid phase extraction and high performance liquid chromatography-tandem mass spectrometry 卢剑, 武中平, 车文军, 洪华, 杨洋 2014 (11):  652-655.  doi: 10.13218/j.cnki.csdc.2014.11.145 摘要 ( 225 )   PDF(868KB) ( 407 )   采用固相萃取(SPE)净化技术和高效液相色谱-串联质谱仪(HPLC-MS/MS),研究并建立了同时测定祛痘化妆品中6种硝基咪唑类药物(甲硝唑、替硝唑、奥硝唑、地美硝唑、洛硝唑和塞克硝唑)的方法。样品用酸化乙腈溶液提取,阳离子固相萃取小柱净化,以体积分数为0.1%甲酸乙腈溶液-体积分数为0.1%甲酸水溶液为流动相,经C18色谱柱梯度洗脱分离,采用HPLC-MS/MS多反应监测模式(MRM)定量检测。结果表明,6种硝基咪唑类药物在质量浓度1.0~50.0 μg·L-1内线性关系良好,相关系数均大于0.999;方法定量限均为0.5 mg·kg-1;在祛痘水和祛痘膏样品中进行3个水平的添加实验,平均回收率为89.7%~108.0%,相对标准偏差(n=6)为2.3%~6.5%。 A method for simultaneous determination of six kinds of nitroimidazole drug (metronidazole (MNZ),tinidazole (TNZ),ornidazole (ONZ),dimetridazole (DMZ),ronidazole (RNZ) and secnidazole (SCZ)) in acne dispelling cosmetics adopting solid phase extraction (SPE) purification technology and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was studied and established.Samples were extracted with acidified acetonitrile solution and the extract was purified with cation resin solid phase exchanging column.Then the purified extract was separated with a C18 column,by gradient elution with acetonitrile and water (containing 0.1% formic acid,volume fraction),and detected by tandem mass spectrometry under multiple reaction monitoring (MRM) mode.The results indicated that good linearity displays when mass concentration of the six kinds of nitroimidazole is within 1.0~50.0 μg·L-1,and all the linear correlation coefficients are higher than 0.999.All the limits of quantification (LOQ) are 0.5 mg·kg-1.The recoveries of six kinds of nitroimidazole when three levels of standard were spiked into samples of acne dispelling cosmetics (both cream type and lotion type) range from 89.7% to 108.0% with RSD (n=6) from 2.3% to 6.5%. 参考文献 | 相关文章 | 计量指标

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高效液相色谱法监控L-焦谷氨酸生产中的脱水反应 Monitoring of dehydration reaction in the production process of L-pyroglutamic acid by HPLC 叶爱英, 徐瑾, 张文雯, 吴芳珍 2014 (11):  656-658.  doi: 10.13218/j.cnki.csdc.2014.11.146 摘要 ( 351 )   PDF(728KB) ( 288 )   研究了用高效液相色谱法监控以L-谷氨酸为原料,在脱水剂作用下脱水合成L-焦谷氨酸的反应进程。采用YMC-Pack Pro C18反相柱(4.6 mm×250 mm×5 μm),以5 mmol·L-1磷酸二氢钾-0.05 mmol·L-1磷酸二氢铵溶液(用磷酸调pH=3.0)/乙腈(体积比为9:1)为流动相,通过标准加入法计算反应液中的L-焦谷氨酸含量。结果表明,该监控方法在0.017 8~0.065 3 g·L-1内线性关系良好(相关系数r=0.998 7);加标平均回收率为99.31%,重复进样的RSD为0.45%。该方法用于实际监控表明,脱水反应可在1 h内完成。 HPLC was applied to monitor the dehydration reaction,in the production process of L-pyroglutamic acid from L-glutamic acid.The chromatography is operated by adopting a YMC-Pack Pro C18 RP column (4.6 mm×250 mm×5 μm) and mobile phase composed of aqueous solution of 5 mmol·L-1 potassium dihydro phosphate and 0.05 mmol·L-1 ammonium dihydro phosphate in combination of acetonitrile with volume ratio of 9:1.The content of L-pyroglutamic acid in reaction solution was determined by the standard spiking method.The results showed that the plot of the content and the peak area displays good linearity in the range of 0.017 8~0.065 3 g·L-1 with r=0.998 7;the average recovery is 99.31%,while the relative standard deviation for repetitions is 0.45%.Based upon this monitoring method,it showed that the dehydration reaction achieves the best condition at reaction time of 1 h. 参考文献 | 相关文章 | 计量指标