当期目录

2018年, 第48卷, 第8期　刊出日期：2018-08-22 上一期    下一期

基础研究

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1-丁基-3-甲基咪唑表面活性离子液体的界面膨胀流变行为研究 Interfacial dilational rheological behavior of (1-butyl-3- methylimidazolium)-based surfactant ionic liquids 侯兆伟,张福玲,伍晓林,孙继超,郑利强 2018 (8):  423-429.  doi: 10.13218/j.cnki.csdc.2018.08.001 摘要 ( 265 )   PDF(5116KB) ( 253 )   研究了1-丁基-3-甲基咪唑十二烷基硫酸盐([bmim][DS])和1-丁基-3-甲基咪唑二(2-乙基己基)磺基琥珀酸酯盐([bmin][AOT]两种表面活性离子液体在正庚烷/水界面的动态界面张力和膨胀特性。比较了[bmim][DS]或[bmin][AOT]和传统表面活性剂十二烷基硫酸钠(SDS)或二(2-乙基己基)磺基琥珀酸酯钠(Na[AOT])之间的膨胀弹性,并且考察了1-丁基-3-甲基咪唑阳离子之间静电相互作用对界面膜特性的影响。另外,通过对比[bmim][DS]和[bmim][AOT]在不同浓度下的膨胀弹性,验证了烷基链数量的改变对界面膨胀流变行为的影响。 The dynamic interfacial tension and dilational properties of 1-butyl-3-methylimidazolium dodecyl sulfate ([bmim][DS]) and 1-butyl-3-methylimidazolium di(2-ethylhexyl) sulfosuccinate ([bmim][AOT]) at n-heptane/water interface were studied.The dilational elasticity of [bmim][DS] or [bmim][AOT] was compared with traditional surfactants (SDS or Na[AOT]).The influence of electrostatic interaction of 1-butyl-3-methylimidazolium cations on the properties of interfacial film was investigated.In addition,by comparing the dilational elasticity at different concentrations of [bmim][DS] and [bmim][AOT],we verified the effects of the change in the number of alkyl chains on the interfacial dilational rheological behavior. 参考文献 | 相关文章 | 计量指标

开发与应用

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利用咪唑啉两性表面活性剂在水相中剥离类水滑石的研究 Study on exfoliation of hydrotalcite-like compounds in aqueous phase with imidazoline amphoteric surfactants 孙慧燕,白雪丽,薛丹丹,黄鑫,张剑,张越 2018 (8):  430-433.  doi: 10.13218/j.cnki.csdc.2018.08.002 摘要 ( 271 )   PDF(6286KB) ( 249 )   采用共沉淀法制备了咪唑啉两性表面活性剂插层的镁铝类水滑石(MgAl-LDHs),再将插层的MgAl-LDHs置于pH=2的水溶液中,使层间呈现阴离子特性的两性表面活性剂转变为阳离子特性,进而通过静电排斥机理,在水相中成功实现MgAl-LDHs层板的剥离。采用X射线衍射、傅里叶变换红外光谱、热重和差示扫描量热分析、透射电子显微镜等技术对样品进行了表征。结果表明,不同分子长度的咪唑啉两性表面活性剂均成功嵌入到MgAl-LDHs层间,且层间距不同。经过插层的MgAl-LDHs能成功剥离,XRD和TEM证实了MgAl-LDHs的分层,同时丁达尔效应证实了胶体的存在。 Imidazoline amphoteric surfactants intercalated MgAl-hydrotalcite-like compounds (MgAl-LDHs) were prepared by co-precipitation method.After placing the MgAl-LDHs in an aqueous solution with pH=2,the amphoteric ions present in the interlayer were converted to cationic,then the exfoliation of MgAl-LDHs layers was successfully achieved in the aqueous phase by electrostatic repulsion.The samples were characterized by X-ray diffraction,fourier transform infrared spectroscopy,thermogravimetry,differential scanning calorimetry,and transmission electron microscopy.The results show that imidazoline amphoteric surfactants with different molecular lengths are successfully embedded between the MgAl-LDHs layers,and the interlayer spacing is different.The intercalated MgAl-LDHs are successfully exfoliated.The results of XRD and TEM have confirmed the stratification of MgAl-LDHs,while the Tyndall effect has confirmed the presence of colloids. 参考文献 | 相关文章 | 计量指标

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基于分子识别和分子印迹的三氯生新型功能材料设计及性能研究 Design and evaluation of functional material for triclosan via molecular recognition and molecular imprinting technology 范维刚,姜莹芳,张亚刚,王璐璐,张乐涛,艾克热木·牙生 2018 (8):  434-438.  doi: 10.13218/j.cnki.csdc.2018.08.003 摘要 ( 230 )   利用分子印迹技术的特异性识别,采用本体热聚合,以酸碱相互作用为基本作用机理,分别以甲基丙烯酸二甲氨基乙酯(DMAEMA)、甲基丙烯酸二乙氨基乙酯(DEAM)、甲基丙烯酸-2-氨基乙基酯盐酸盐(AMA盐酸盐)、4-乙烯基吡啶(4-VP)和甲基丙烯酸(MAA)为功能单体,乙二醇二甲基丙烯酸酯(EGDMA)和二乙烯基苯(DVB)为交联剂,偶氮二异丁腈(AIBN)为引发剂,乙腈为溶剂设计合成了三氯生(TCS)的分子印迹聚合物(MIPs)。吸附结果表明,其中DEAM是TCS的最佳功能单体,吸附率达到了78.5%,印迹因子达到了1.7,用DEAM作为功能单体合成的MIPs对TCS的选择性实验结果显示,对TCS的吸附容量明显高于其结构类似物,对TCS的吸附实验结果显示,5次回收后重复利用,吸附容量仅降低了5.1%,表明该MIPs可以重复使用多次。 The working mechanism of molecularly imprinted polymers (MIPs) for triclosan (TCS) is based on acid-base interaction.The designed MIPs were prepared by thermal bulk polymerization using DMAEMA,DEAM,hydrochloride of AMA,4-VP and MAA as functional monomers,EGDMA and DVB as cross-linkers,AIBN as initiator and acetonitrile as solvent.Adsorption study shows that the MIPs made with DEAM achieve highest adsorption percentage of 78.5% and imprinting factor of 1.7.The selective binding experiments show that DEAM-MIPs show high selectivity to TCS over other structural analogues.Adsorption experiments on TCS by MIPs show that after 5 times of recovery,the adsorption capacity only drops by 5.1%,indicating that the MIPs can be reused multiple times. 参考文献 | 相关文章 | 计量指标

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烷基改性有机硅弹性体微球的制备及表征 Preparation and characterization of alkyl-modified silicone elastomer microspheres 吕锡明,杨成 2018 (8):  439-443.  doi: 10.13218/j.cnki.csdc.2018.08.004 摘要 ( 418 )   PDF(5073KB) ( 274 )   以1-十二烯和含氢硅油(PMHS)为原料,通过硅氢加成反应制备得到不同烷基接枝率的烷基改性含氢硅油(R-PMHS)。以R-PMHS和乙烯基封端硅油(Vi-PDMS)为油相,亲水性纳米SiO2颗粒和少量十六烷基三甲基溴化铵(CTAB)为乳化剂,采用Pickering乳液聚合法制备烷基改性有机硅弹性体微球。结果表明,CTAB水溶液浓度为2×10-4 mol/L、油/水质量比为1∶1、纳米SiO2占油相质量分数为4%、硅氢键(Si-H)与乙烯基(Vinyl)摩尔比为2∶1时得到的乳液稳定性和微球的形貌最好。吸油量测试表明,随着烷基接枝率增加有机硅弹性体微球的亲油性不断增大。 Alkyl-modified polymethylhydrosiloxane (R-PMHS) with different percent grafting of alkyls was prepared by hydrosilylation of 1-dodecene and polymethylhydrosiloxane (PMHS).The alkyl-modified silicone elastomer microspheres were prepared by Pickering emulsion polymerization with R-PMHS and vinyl-terminated polydimethylsiloxane (Vi-PDMS) as oil phase and the hydrophilic nano-SiO2 particles and a small amount of cetyltrimethylammonium bromide (CTAB) as emulsifiers.The results show that the most stable emulsion together with the best morphology of microspheres were obtained when the concentration of CTAB is 2×10-4 mol/L,the mass ratio of oil to water is 1∶1,the mass fraction of nano-SiO2 to oil phase is 4% and the molar ratio of silicon-hydrogen bond (Si-H) to vinyl is 2∶1.The oil absorption results show that the lipophilicity of these silicone elastomer microspheres increases with the increase of percent grafting of alkyls. 参考文献 | 相关文章 | 计量指标

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不同介质溶液对维生素C稳定性的影响研究 Study on the effect of different medium solutions on the stability of Vitamin C 陈惠芳,蒋新元,陈介南,许琼文,孟浩亮 2018 (8):  444-449.  doi: 10.13218/j.cnki.csdc.2018.08.005 摘要 ( 448 )   PDF(4418KB) ( 282 )   利用紫外分光光度法研究了无机盐、羧甲基纤维素钠、 β-环糊精和聚乙二醇等介质溶液中维生素C的稳定性,并探索了上述介质溶液延缓维生素C被氧化的作用机理。结果表明,氯化镁、氯化钾、氯化钠、羧甲基纤维素钠均能较显著地提高维生素C的稳定性,而羧甲基纤维素钠对人体安全、使用量很少且效果显著,可广泛应用在化妆品、食品、医药等领域用以保护维生素C的稳定性。聚乙二醇、 β-环糊精与维生素C的混合溶液中起始溶氧量与空白维生素C溶液相近且随时间延长下降很明显,而氯化钠、羧甲基纤维素钠和维生素C的混合溶液中起始溶氧量则远低于空白维生素C溶液并随时间延长下降很慢,这些现象与上述介质对维生素C的保护效果是一致的。介质溶液中起始溶氧量的高低及下降速度快慢影响了维生素C的稳定性,无机盐离子种类和浓度影响溶液中溶氧量,而羧甲基纤维素钠、聚乙二醇、 β-环糊精等溶液的相对黏度则对溶氧量存在影响。 The stability of Vitamin C in different medium solutions such as inorganic salts,sodium carboxymethyl cellulose, β-cyclodextrin and polyethylene glycol was studied by ultraviolet spectrophotometry,and the mechanism of the above mediums retarded the oxidation of Vitamin C was also explored.The results show that magnesium chloride,potassium chloride,sodium chloride and sodium carboxymethyl cellulose can significantly improve the stability of Vitamin C.While the sodium carboxymethyl cellulose is safe,less dosage and has significant effect to protect Vitamin C,it can be widely used in cosmetics,food,medicine and other fields to protect the stability of Vitamin C.The amount of initial dissolved oxygen content in the mixed solution of polyethylene glycol, β-cyclodextrin and Vitamin C is similar to that of the blank Vitamin C solution,and it significantly decreases with time.However,the amount of initial dissolved oxygen content in the mixed solution of sodium chloride,carboxymethyl cellulose and Vitamin C is much lower than that of the blank Vitamin C solution and it decreases very slowly with time.These phenomena are consistent with the protective effect of the above medium solutions on Vitamin C.The level of initial dissolved oxygen content in the medium solutions and the speed of decline affect the stability of Vitamin C.The type and concentration of inorganic salt ions affect the amount of dissolved oxygen content in the solution,while the solution viscosity has the effect on the dissolved oxygen content in water-soluble polymer solutions such as sodium carboxymethyl cellulose,polyethylene glycol and β-cyclodextrin. 参考文献 | 相关文章 | 计量指标

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一种复方中草药提取液的护肤功效研究 Study on skincare efficacy of compound extract from Chinese herbal medicines 刘芳,徐勇威,王珊珊,龚盛昭 2018 (8):  450-456.  doi: 10.13218/j.cnki.csdc.2018.08.006 摘要 ( 612 )   PDF(5646KB) ( 323 )   采用体外实验和人体实验相结合方法,对5种中草药为原料制成的复方提取液进行美白、抗衰老、抗敏舒缓功效研究,并对其刺激性进行评价。结果表明,复方提取液的刺激性分级为无刺激性,具有较强的抑制酪氨酸酶活性、清除DPPH/羟基/超氧阴离子自由基及抑制透明质酸酶活性的能力;使用含复方提取液的乳液4周后,能显著减少皮肤黑色素含量和降低皮肤紫外斑、黄褐斑、皱纹、纹理分值;此外,含复方提取液的乳液能够降低乳酸刺痛程度。上述结果说明该复方中草药提取液使用安全性高,具有较好的美白、抗衰老、抗敏舒缓功效。 A combination of in vitro experiments and human efficacy evaluation were used to assess the whitening,anti-aging and anti-allergic soothing efficacy and the irritation of a compound extract which was obtained from 5 kinds of Chinese herbal medicines.The results show that the compound extract is classified as non-irritation substance.Besides,it has strong ability to inhibit tyrosinase activity,scavenge DPPH/hydroxyl/superoxide anion radicals and inhibit hyaluronidase activity.After 4 weeks of using the emulsion containing the compound extract,it can significantly reduce skin melanin content and decrease the scores of skin UV spots,chloasma,wrinkle and texture.In addition,this emulsion containing the compound extract can effectively relieve the tingling caused by lactic acid.The above results indicate that this compound extract is a safe and effective cosmetics raw material which has good whitening,anti-aging and anti-allergic soothing efficacy. 参考文献 | 相关文章 | 计量指标

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口腔长效抑菌缓释剂的制备与研究 Preparation and study of oral sustained-release formulation with long-acting bacteriostasis 陈伟才,易丹,李淑钰,张利萍,蒋庆 2018 (8):  457-461.  doi: 10.13218/j.cnki.csdc.2018.08.007 摘要 ( 309 )   PDF(3554KB) ( 271 )   通过测定多种牙膏常用的抑菌药物的最低抑菌浓度(MIC),发现西吡氯铵(CPC)和氯己定对变异链球菌和牙龈卟啉单胞菌均具有强烈的抑制作用,其MIC均低于1 mg/L。利用三乙酰基-β-环糊精(TA-CD)和乙基纤维素(EC)对CPC进行包裹,喷雾干燥制样,得到的载药颗粒具有明显的“暴释”现象,加入硬脂酸(SA)后,载药颗粒表现出更好的缓释效果。另外,在载药颗粒中添加一定量的聚乙烯醇(PVA),可以明显提升载药颗粒刷牙后在口腔的附着率,当PVA的质量分数为20%时,载药颗粒的附着率最高,达到19.1%。利用混合菌生物膜对DLP-7载药颗粒和CPC进行抑菌评价,实验结果表明,随着时间延长,载药颗粒抑菌率不断增加,4 h后其抑菌率要明显高于CPC对于生物膜的抑菌率,即DLP-7载药颗粒体现出长效的抑菌效果。 By measuring the minimal inhibitory concentration (MIC) of various antibacterial drugs commonly used in toothpaste,it is found that both cetylpyridinium chloride (CPC) and chlorhexidine have strong bacteriostatic effect on Streptococcus mutans and Porphyromonas gingivalis with the MIC below 1 mg/L.The CPC was coated with triacetyl-β-cyclodextrin (TA-CD) and ethyl cellulose (EC) and particles were prepared by spray drying.The drug-loaded particles had obvious “burst release” phenomenon,and it showed better sustained release effect after adding stearic acid (SA).In addition,the adhesion rate of the drug-loaded particles can be significantly improved after brushing,when certain amount of polyvinyl alcohol (PVA) was added.When the mass fraction of PVA is 20%,the adhesion rate of the drug-loaded particles is the highest,reaching 19.1%.The mixed bacterium biofilm was used to evaluate the bacteriostasis of drug-loaded particle (DLP-7) and CPC.The results show that the relative inhibition rate of drug-loaded particles increases continuously over time.After 4 h,the relative inhibition rate of DLP-7 is higher than CPC,which means that DLP-7 shows long-acting bacteriostasis. 参考文献 | 相关文章 | 计量指标

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橄榄苦甙牙膏的开发及其功效研究 Study on the development and efficacy of oleuropein toothpaste 刘庆刚 2018 (8):  462-465.  doi: 10.13218/j.cnki.csdc.2018.08.008 摘要 ( 288 )   PDF(2802KB) ( 255 )   通过橄榄苦甙在不同牙膏配方中的实验研究确定了橄榄苦甙牙膏的最佳应用方案,产品中橄榄苦甙含量通过高温稳定性进行考察。体外抑菌实验及临床验证结果证明含有一定量橄榄苦甙的牙膏具有良好的抑菌作用,并对加入橄榄苦甙牙膏的药理作用与毒理作用进行了试验研究。 Through the experimental study of oleuropein in different toothpaste formulations,the optimal application scheme was determined.The content of oleuropein in toothpaste was investigated by high temperature stability test.The in vitro bacteriostasis experiment and clinical trial results prove that the toothpaste containing a certain amount of oleuropein has good bacteriostasis effect.And the pharmacological and toxicological effects of the toothpaste containing oleuropein were studied. 参考文献 | 相关文章 | 计量指标

分析与检测

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高效液相色谱法测定化妆品中苯扎氯铵含量的不确定度评定 Evaluation of uncertainty in the determination of benzalkonium chloride in cosmetics by HPLC 王涛,李卓,贾寒冰,孙晓,田仁芳,荀英 2018 (8):  466-471.  doi: 10.13218/j.cnki.csdc.2018.08.009 摘要 ( 363 )   PDF(4169KB) ( 287 )   对《化妆品安全技术规范》(2015年版)中高效液相色谱法测定苯扎氯铵3种物质(即十二烷基二甲基苄基氯化铵(C12)、十四烷基二甲基苄基氯化铵(C14)和十六烷基二甲基苄基氯化铵(C16))含量进行了不确定度评定,建立了数学模型,考察了不确定度的来源并给出了量化结果,计算出合成标准不确定度和扩展不确定度。结果表明,当取置信概率为95%,包含因子k=2,被测化妆品中苯扎氯铵C12,C14和C16含量分别为0.045%,0.048%和0.010%时,其标准扩展不确定度分别为0.027%,0.029%和0.006%。指出了测量不确定度的主要来源,并提出了改进方法。 Uncertainties from the determination procedure of three substances of benzalkonium chloride (dodecyldimethylbenzylammonium chloride (C12),tetradecyldimethylbenzylammonium chloride (C14) and hexadecyldimethylbenzylammonium chloride (C16) in Safety and Technical Standards for Cosmetics (2015 Edition) by high performance liquid chromatography (HPLC) were assessed.The mathematical model was established,and the source of uncertainty was investigated and quantified.The combined standard uncertainty and expanded uncertainty were calculated.The results show that the expanded uncertainties are 0.027%,0.029% and 0.006% (95% confidence level,k=2) when the mass fraction of benzalkonium chloride (C12,C14 and C16 ) in cosmetics are 0.045%,0.048% and 0.010%,respectively.The main sources of the uncertainty are analyzed,and improved method is introduced. 参考文献 | 相关文章 | 计量指标

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高效液相色谱-串联质谱法测定香水中24种香料类过敏原物质残留量 Determination of 24 allergens in perfume with high performance liquid chromatography tandem mass spectrometry 王玉健,梁振纲,符灵梅,董存柱 2018 (8):  472-477.  doi: 10.13218/j.cnki.csdc.2018.08.010 摘要 ( 320 )   PDF(4399KB) ( 264 )   建立了高效液相色谱-串联质谱法同时测定香水中24种香料类过敏原物质残留量的方法。样品经乙腈提取,以电喷雾离子源(ESI)、多反应监测模式扫描,外标法定量。结果显示,24种香料类过敏原物质在1.0~5.0 mg/L范围内线性关系良好,仪器检出限为1.0 mg/L,方法的检测限为5.0 mg/kg,定量限为15.0 mg/kg,添加水平为5,10和20 mg/kg时,24种香料类过敏原物质的平均回收率为85.9%~110.0%,精密度为5.5%~12.0% (n=10)。 A method of simultaneous determination of 24 allergens in perfume was established with high performance liquid chromatography tandem mass spectrometry.The target compounds were extracted with acetonitrile and determined with HPLC-MS/MS (MRM mode,ESI) with external standard method.The results show that,good linear relationship between concentration and peak area ratio is obtained in the range of 1.0~5.0 mg/L for the 24 allergens.The instrument detection limit is 1.0 mg/L and the method detection limit is 5.0 mg/kg.The limit of quantitation (LOQ) is 15.0 mg/kg.The average recoveries of 24 allergens are 85.9%~110.0% at spiked levels of 5,10 and 20 mg/kg with relative standard derivations (RSDs) of 5.5%~12.0% (n=10). 参考文献 | 相关文章 | 计量指标

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柱前衍生-高效液相色谱法测定化妆品中氯乙醛和戊二醛 Determination of chloroacetaldehyde and glutaral in cosmetics by pre-column derivatization-high performance liquid chromatography 林文进,寻知庆,黄金凤,郭新东,罗晓茵,叶嘉荣 2018 (8):  478-482.  doi: 10.13218/j.cnki.csdc.2018.08.011 摘要 ( 395 )   PDF(3346KB) ( 255 )   建立了化妆品中氯乙醛和戊二醛的柱前衍生-高效液相色谱(HPLC)分析方法。样品使用体积分数为50%的乙腈溶液提取,2,4-二硝基苯肼柱前衍生,经RRHD C18色谱柱(2.1 mm×50 mm,1.7 μm)分离后,高效液相色谱-二极管阵列检测器检测,以保留时间和紫外吸收光谱定性,外标法定量。结果表明,氯乙醛和戊二醛衍生物在质量浓度0.05~5.0 mg/L范围内呈现良好的线性关系,相关系数均大于0.999 4;方法检出限和定量限分别为1.0和3.0 mg/kg。样品加标回收率为89.5%~106.1%,相对标准偏差(RSDs,n=6)为1.9%~6.6%。该方法适用于化妆品中氯乙醛和戊二醛的测定。 A pre-column derivatization-high performance liquid chromatography (HPLC) method was established for the determination of chloroacetaldehyde and glutaral in cosmetics.The samples were extracted with 50% acetonitrile solution (in volume ratio),derivatized with 2,4-dinitrophenylhydrazine,separated by RRHD C18 column (2.1 mm×50 mm,1.7 μm) and detected by HPLC-diode array detector.The retention time and UV absorption spectra were adopted for qualitative and an external standard method was used to quantify.Under the optimal conditions,the results show that chloroacetaldehyde and glutaral have good linear relationship in the range of 0.05-5.0 mg/L with the correlation coefficients greater than 0.999 4.The detection limit and quantification limit of the method are 1.0 and 3.0 mg/kg,respectively.The recoveries of spiked samples are ranged from 89.5% to 106.1% and the relative standard deviations (RSDs,n=6) are between 1.9% and 6.6%.The method is suitable for the determination of chloroacetaldehyde and glutaral in cosmetics. 参考文献 | 相关文章 | 计量指标