日用化学工业（中英文）

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香兰素基非离子表面活性剂的动态表面张力与气/液界面吸附行为
Dynamic surface tension and adsorption behavior of vanillin-based nonionic surfactants at gas-liquid interface

翟功勋, 丁凤美, 邢志奇, 周翔

2018 (6): 303-307. doi: 10.13218/j.cnki.csdc.2018.06.001

摘要 ( 259 )

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通过最大气泡压力法测定香兰素基聚氧乙烯醚(VAEO)的动态表面张力,利用Word-Tordai方程研究其在气/液界面的吸附行为。结果表明,质量浓度低于临界胶束浓度(cmc)时,VAEO在吸附前期为扩散控制吸附,在吸附后期为混合动力控制吸附;质量浓度大于cmc时,为混合动力控制吸附,胶束不影响吸附行为。VAEO₁₀和VAEO₂₀的扩散系数D的数量级为10^-11 m²/s,比文献报道的壬基酚聚氧乙烯醚(NPEO₉)低一个数量级。 The dynamic surface tension of vanillin-based polyoxyethylene ethers (VAEO) was measured by the maximum bubble pressure method.The adsorption mechanism of surfactants at gas-liquid interface was studied by using Word-Tordai equation.The results show that when the mass concentration of VAEO is below critical micelle concentration (cmc),the adsorption of VAEO obeys the mechanisms of diffusion controlled adsorption and mixed diffusion-kinetic controlled adsorption,respectively,at the early stage and the later stage of adsorption.When the mass concentration is above cmc,the adsorption mechanism is mixed diffusion-kinetic controlled adsorption,where the micelles do not affect the adsorption behavior.The magnitude of diffusion coefficients of VAEO₁₀ and VAEO₂₀ are 10^-11 m²/s,which are lower than the NPEO₉s reported in literature.

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水杨酸钠对DTAB/PAM复合体系自组装行为的影响
Effects of sodium salicylate on the self-assembly behavior of DTAB/PAM mixed system

陈雨嘉, 刘嘉希, 朱倩倩, 胡松青, 孙霜青, 王秀民

2018 (6): 308-313. doi: 10.13218/j.cnki.csdc.2018.06.002

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通过粗粒度分子动力学模拟的方法研究了水杨酸钠(NaSal)对聚丙烯酰胺(PAM)与表面活性剂十二烷基三甲基溴化铵(DTAB)复合体系自组装行为的影响。结果表明,随着添加的NaSal浓度增大,DTAB/PAM聚集体经历了球形-棒状-球形的结构变化,且吸附到聚合物链上的DTAB分子数目先增大后减小。在DTAB/PAM聚集体中,聚合物PAM分子链位于DTAB胶束疏水内核与亲水层的交界处,有机盐Sal^-插入到胶束内部。聚合物分子链的回转半径(Rg)随时间的变化以及聚集体中表面活性剂数目随时间的变化过程均可以分为3个阶段,且形成尺寸较大的DTAB/PAM聚集体需要更长的时间。 The effects of sodium salicylate (NaSal) on the self-assembly behavior of the mixed system of polyacrylamide (PAM) and dodecyltrimethylammonium bromide (DTAB) were studied by coarse-grained molecular dynamics simulation.The results indicate that,with the increase of NaSal concentration,the aggregates of DTAB/PAM undergo a shape transition from sphere to rod then to sphere,and the number of DTAB molecules adsorbed onto HPAM chains first increases and then decreases.As for the DTAB/PAM aggregate,the PAM chain is located at the interface between the hydrophobic core and the hydrophilic layer of the DTAB micelle,and the Sal^- ions are inserted into the interior of the micelle.The variations with time of the polymer chains Rg and the number of surfactant molecules in the aggregate can be both divided into three stages.The formation of larger DTAB/PAM aggregates needs longer time.

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化妆品功效评价(Ⅵ)——化妆品人体功效评价的实验设计
Efficacy evaluation of cosmetics (Ⅵ) Experimental design of cosmetics human efficacy evaluation

盘瑶, 赵华

2018 (6): 314-321. doi: 10.13218/j.cnki.csdc.2018.06.003

摘要 ( 623 )

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概述了化妆品人体功效评价实验设计的概念、基本要素和基本原则,介绍了常用实验设计类型和实验设计要点,提供了人体功效评价实验方案设计的思路,有助于提高研究者制定实验设计方案的水平。 The concept,basic elements,and basic principles of experimental design of cosmetics human efficacy evaluation were summarized.The commonly used types and key points of experimental design were introduced.The new idea of the design of cosmetics human efficacy evaluation protocol was proposed,in order to improve the ability of researchers to make a reliable experiment protocol.

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油酸甲酯乙氧基化物耐酸耐碱性研究
Study on the acid and alkali resistance of oleic acid methyl ester ethoxylate

张勇, 孙永强, 丁莉荣, 周婧洁, 孙晋源, 梁慧斌

2018 (6): 322-325. doi: 10.13218/j.cnki.csdc.2018.06.004

摘要 ( 324 )

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将油酸甲酯乙氧基化物(OMEE)作为研究对象,通过FT-IR鉴定结构;分别采用国标法和质量法定性、定量测定FMEE和OMEE耐酸耐碱性。由实验结果可知,OMEE与常规饱和脂肪酸甲酯乙氧基化物(FMEE)在结构上存在碳碳双键的差异;国标法不适用于脂肪酸甲酯乙氧基化物耐酸耐碱性的测定;在任意pH值,OMEE的水解率始终高于FMEE;在pH=13时,FMEE和OMEE水解速率最快,且在170 h时OMEE水解完全;FMEE在pH=2~9、500 h时水解率仍小于20%;OMEE在pH小于13时,水解率受pH和时间影响较小。 Oleic acid methyl ester ethoxylate (OMEE) was characterized by FT-IR.The acid and alkali resistance of fatty acid methyl ester ethoxylate (FMEE) and OMEE were measured qualitatively and quantitatively by national standard method and mass method,respectively.The experimental results show that,the structure of OMEE is different from that of conventional saturated FMEE because of the presence of carbon-carbon double bond.The national standard method is not suitable for the determination of acid or alkali resistance of FMEE.The hydrolysis rate of OMEE is always higher than that of FMEE at any pH.The hydrolysis of both FMEE and OMEE are the fastest at pH 13,and OMEE has been hydrolyzed completely at 170 h.At pH 2~9,the hydrolysis rate of FMEE is still less than 20% during the period of 500 h.In additon,the hydrolysis rate of OMEE has been little affected by either pH or time when the pH is less than 13.

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黄皮果果核挥发油抗UV致小鼠皮肤光老化损伤的实验研究
Study on the effect of essential oil from fruit kernel of Wampee against UV-induced skin photoaging in mice

彭志红, 吴科锋, 黄燕霞, 廖雪华, 欧阳佩佩, 李文德

2018 (6): 326-329. doi: 10.13218/j.cnki.csdc.2018.06.005

摘要 ( 318 )

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通过水蒸气蒸馏法和冷冻结晶法对黄皮果果核挥发油进行提取和分离,将所得黄皮果果核挥发油涂于去毛KM小鼠背部,再进行UVA/UVB联合照射,从皮肤表观评价得分及HE染色结果对其抗光老化作用进行评价。结果表明,1.9%的维生素E供试液作为阳性对照药,能起到显著的抗皮肤光老化作用,2.5%,5%和10%的黄皮果果核挥发油供试液可起到抗UV所致真皮病变的作用,5%和10%时可改善UV照射所引起的表皮增厚及皱褶产生等表皮病变。 The essential oil from fruit kernel of Wampee was extracted by steam distillation and separated by frozen crystallization.Then the essential oil was applied to the back of hairless KM mice.Score of skin clinical observation and histopathological examination were performed to evaluate the anti-photoaging effects after UVA/UVB combined irradiation.Results show that 1.9% Vitamin E as the positive control plays a significant role in anti-photoaging,The essential oil from fruit kernel of Wampee at the dose of 2.5%,5% and 10% can play a role in resisting UV-induced dermis lesions ,and can improve UV-induced epidermal lesions like epidermal thickening and wrinkle formation at 5% and 10%.

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油茶籽油不皂化物的提取与抗氧化性研究
Study on extraction of unsaponifiable matter in camellia oil and its antioxidant activity

周振宇, 杨成, 蔡春辉

2018 (6): 330-335. doi: 10.13218/j.cnki.csdc.2018.06.006

摘要 ( 292 )

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以油茶籽油为原料,通过皂化-己烷萃取法提取其不皂化物。通过气相色谱-质谱联用技术(GC-MS)对油茶籽油不皂化物的组成进行了分析,并通过1,1-二苯基-2-三硝基苯肼(DPPH)法、三价铁离子还原力(FRAP)法以及细胞抗氧化(CAA)法对其抗氧化性能进行了测定,并与α-生育酚进行了比较。结果表明,通过皂化-己烷萃取法得到的油茶籽油不皂化物主要含有烃类、三萜醇以及植物甾醇;油茶籽油不皂化物的DPPH自由基清除率可达到95%,EC₅₀为1.9 g/L;油茶籽油不皂化物具有一定的Fe³⁺还原能力,在质量浓度为5 g/L时,FRAP值可达170;油茶籽油不皂化物能够进入细胞并对2,2-偶氮(2-甲基丙基脒)二盐酸盐(ABAP)诱导的细胞内活性氧水平升高具有抑制作用,质量浓度为100 mg/L时CAA值可达36.6。 Camellia oil was used as raw material to extract unsaponifiable matter (USM) by saponification-hexane extraction method.The compositions of USM in camellia oil were analyzed by gas chromatography-mass spectrometry (GC-MS),and DPPH radical-scavenging assay,ferric reducing-antioxidant power (FRAP) test and cellular antioxidant activity assay (CAA) were applied to determine their antioxidant activity in comparison with α-tocopherol.Results indicate that the compositions of USM in camellia oil obtained by saponification-hexane extraction are mainly hydrocarbon,triterpene alcohol and phytosterol.The DPPH free radical scavenging rate of USM in camellia oil is 95%,and the EC₅₀ is 1.9 g/L.USM in camellia oil has certain ability to reduce Fe³⁺,and the FRAP value is 170 at the mass concentration of 5 g/L.USM in camellia can enter the HSF cells and inhibit the ABAP-induced intracellular reactive oxygen species formation.The CAA value is up to 36.6,when the mass concentration of USM is 100 mg/L.

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单分散聚甲基丙烯酸甲酯微球为模板制备大孔氧化铝材料
Preparation of macroporous aluminium oxide by using mono-dispersed PMMA microspheres as templates

张勇, 孔庆岚, 刘芝平, 延姗姗, 于峰

2018 (6): 336-340. doi: 10.13218/j.cnki.csdc.2018.06.007

摘要 ( 318 )

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以过硫酸铵为引发剂、十二烷基硫酸钠为乳化剂、甲基丙烯酸甲酯为单体,通过乳液聚合制备了聚甲基丙烯酸甲酯(PMMA)乳胶微球。研究显示,通过改变合成体系中乳化剂用量可对合成的PMMA微球的粒径进行有效调控,并得到了粒径分布在200~300 nm的PMMA微球;通过破乳沉降法加速PMMA微球的自组装,得到紧密堆积的PMMA微球胶体模板。将溶解在乙醇(经盐酸酸化)中的异丙醇铝溶液填充到组装好的PMMA胶体模板剂的空隙中,通过焙烧去除模板制得大孔氧化铝材料,在950 ℃焙烧3 h得到了规整大孔γ-Al₂O₃;扫描电镜和透射电镜结果表明所得材料孔道丰富,为三维有序大孔材料。 Mono-dispersed polymethyl methacrylate (PMMA) latex microspheres were prepared by emulsion polymerization using ammonium persulfate as initiator,sodium dodecyl sulfate as emulsifier and methyl methacrylate as monomer.The results show that the particle size of the as-synthesized PMMA microspheres can be effectively controlled and adjusted by changing the content of emulsifier.The PMMA microspheres with diameter distribution of 200~300 nm were obtained.The self-assembly of PMMA microspheres was accelerated by demulsification sedimentation method so as to obtain a tightly packed PMMA microsphere colloidal template.The solution of aluminum isopropoxide dissolved in ethanol (acidified by hydrochloric acid) was filled into the interspaces of the PMMA colloidal template.The macroporous material of alumina was then obtained by roasting the template.γ-Al₂O₃ three-dimensionally ordered macroporous material (3DOM) was obtained by calcination at 950 ℃ for 3 h.The results of SEM and TEM show that the material is 3DOM which has many porous channels.

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苄基接枝海藻酸衍生物对TiO₂纳米粒分散稳定性的影响
Effects of benzyl-grafted alginate derivative on the dispersion stability of TiO₂ nanoparticles

冯美西, 颜慧琼, 陈秀琼, 林良泉, 杨正, 林强

2018 (6): 341-347. doi: 10.13218/j.cnki.csdc.2018.06.008

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以溴化苄为疏水改性剂,采用双分子亲核取代反应(SN2)制得苄基接枝海藻酸衍生物(BAD)。通过动态光散射技术,考察了在不同pH和离子强度下BAD对TiO₂纳米粒水悬浮液分散稳定性的影响。并采用红外光谱和扫描电镜对BAD/TiO₂纳米粒复合物的官能团和表面形貌进行了测试。结果表明,通过SN2反应成功地合成了具有胶体性能的BAD。BAD胶束的平均水动力学粒径(d_H)大小为423.4 nm,Zeta电位值为-27.4 mV,表现出较好的胶体性能。在不同pH下,BAD的吸附可提高TiO₂纳米粒的带电性,使其Zeta电位均低于-30 mV,而且其d_H相比单一的TiO₂纳米粒显著减小。在不同离子强度下,BAD可明显削弱反离子对TiO₂纳米粒静电屏蔽作用的影响,使TiO₂纳米粒的团聚行为大大降低,d_H显著减小。BAD分子链不仅能够提高TiO₂颗粒间的静电斥力,而且还能提供有效的空间位阻,提高TiO₂纳米粒在不同pH和离子强度下的分散稳定性。红外和扫描电镜分析结果表明,BAD和TiO₂纳米粒主要通过氢键作用来实现BAD在TiO₂纳米颗粒上的吸附,从而提高TiO₂纳米颗粒间的空间位阻作用使其稳定分散。 Benzyl-grafted alginate derivative (BAD) was prepared by bimolecular nucleophilic substitution reaction (SN2) using benzyl bromide as a hydrophobic modifier.The effects of BAD on the dispersion stability of aqueous suspension of TiO₂ nanoparticles at different pH and ionic strength were investigated by dynamic light scattering.Additionally,the functional groups and morphology of BAD/TiO₂ nanoparticle composite were measured by fourier transform infrared spectroscopy and scanning electron microscopy.The experimental results show that the colloidal BAD is successfully synthesized by SN2 reaction.The average hydrodynamic size (d_H) of BAD micelles is 423.4 nm and the Zeta potential is-27.4 mV,which exhibits good colloidal properties.At different pH,the adsorption of BAD can enhance the chargeability of TiO₂ nanoparticles,which makes their Zeta potential to be lower than -30 mV and their d_H to be significantly lower than that of single TiO₂ nanoparticles.At different ionic strength,BAD can obviously weaken the electrostatic shielding effect of counterions on TiO₂ nanoparticles,which makes the agglomeration behavior of TiO₂ nanoparticles to be greatly reduced and their d_H to be significantly decreased.The molecular chain of BAD can not only enhance the electrostatic repulsion among TiO₂ particles,but also provide effective steric hindrance,which improves the dispersion stability of TiO₂ nanoparticles at different pH and ionic strength.The results of infrared spectroscopy and scanning electron microscopy indicate that the adsorption of BAD on TiO₂ nanoparticles is achieved mainly through the hydrogen bonding between BAD and TiO₂ nanoparticles,which has enhanced the steric hindrance among TiO₂ nanoparticles and thus makes them dispersed stably.

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胶束十二烷基硫酸钠增敏荧光法测定银杏叶片槲皮素含量
Determination of quercetin in Ginkgo leaves tablets by micellar SDS enhanced fluorimetry

陈金娥, 张海容

2018 (6): 348-351. doi: 10.13218/j.cnki.csdc.2018.06.009

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建立了银杏叶片中测定槲皮素含量的十二烷基硫酸钠(SDS)增敏荧光新方法。实验考察了表面活性剂种类、用量及pH等外界条件对槲皮素荧光强度的影响。结果表明,所选用的SDS、十六烷基三甲基溴化铵(CTMAB)、曲拉通X-100(Triton X-100)、 β-环糊精(β-CD)4种有序介质,SDS在碱性(pH=9.12)介质中对槲皮素荧光增敏效果最好,在最大激发波长464 nm、最大发射波长542 nm处有强荧光发射峰。在pH=9.12、SDS浓度为1.5×10^-2 mol/L优化实验条件下,体系荧光强度与槲皮素含量成线性关系,线性范围为2~14 μg/mL,检出限为0.16 ,RSD为1.56%。本方法用于4种银杏叶片中槲皮素含量测定,结果满意。 A new method for the determination of quercetin in Ginkgo leaves tablets was established by sodium dodecyl sulfate (SDS) enhanced fluorimetry.The effects of external conditions,such as the type and amount of surfactant and pH on the fluorescence intensity of quercetin were investigated.Results show that among the four kinds of ordered media,i.e.,SDS,CTMAB,Triton X-100 and β-CD,the fluorescence intensity of quercetin is greatly enhanced in SDS solution under alkaline condition (pH=9.12) with a strong fluorescence emission peak at λ_ex/λ_em=464/542 nm.Under the optimal experimental conditions of pH=9.12 and SDS concentration of 1.5×10^-2 mol/L the linear relationship between fluorescence intensity and concentration of quercetin is kept in the range of 2-14 μg/mL with the detection limit of 0.16 μg/L and RSD of 1.56%.The method has been applied to the determination of quercetin in four kinds of Ginkgo leaves tablets with satisfactory results.

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气相色谱法测定化妆品用原料聚乙烯醇中甲醇含量
Determination of methanol in polyvinyl alcohol used in cosmetics by gas chromatography

杨铭, 张丽华, 胡丹, 王晨蕾, 任承方

2018 (6): 352-355. doi: 10.13218/j.cnki.csdc.2018.06.010

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建立了气相色谱法测定化妆品用原料聚乙烯醇(固体)中甲醇含量的方法。研究发现顶空法较蒸馏法、直接稀释法更适合用于测定化妆品用原料聚乙烯醇中甲醇含量。分别考察了溶剂和盐析剂对测定结果的影响,发现最佳的溶剂和盐析剂分别为10 mL水和0.5 g氯化钠。结果表明甲醇质量浓度在10~1 000 mg/L范围内线性关系良好,相关系数可达0.999 5,其回收率为92.6%~104.8%,相对标准偏差在1.2%~6.5%之间,检出限为5 mg/L。实验结果证明,该方法适用于化妆品用原料聚乙烯醇中甲醇含量的检测。 A gas chromatography method was established for the determination of methanol in polyvinyl alcohol used in cosmetics.It is found that headspace method is more suitable than distillation method and direct dilution method to determine the methanol in polyvinyl alcohol used in cosmetics.The factors of solvent and salting-out agent were investigated and the appropriate conditions are 10 mL water and 0.5 g sodium chloride,respectively.Results indicate that the linear relationship of methanol in the range of 10-1 000 mg/L is good,with correlation coefficient of 0.999 5.The recoveries are ranged from 92.6% to 104.8%,while the relative standard deviations are ranged from 1.2% to 6.5% and the detection limit is 5 mg/L.The results prove that this method is suitable for the determination of methanol in polyvinyl alcohol used in cosmetics.

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固相萃取-气相色谱-质谱法同时测定化妆品中多环芳烃和邻苯二甲酸酯类物质
Simultaneous determination of polycyclic aromatic hydrocarbons and phthalic acid esters in cosmetics by GC-MS with solid-phase extraction

张瑞瑞, 汪晨霞, 李秀英, 杜伟锋, 郭新东

2018 (6): 356-362. doi: 10.13218/j.cnki.csdc.2018.06.011

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建立了固相萃取(SPE)-GC-MS法同时测定化妆品中的16种多环芳烃(PAHs)和17种邻苯二甲酸酯类(PAEs)的分析方法。样品经乙腈超声萃取后,经PSA/Slica玻璃柱净化,以Agilent Select PAH色谱柱分离,气相色谱-质谱法选择离子(SIM)监测测定。16种PAHs和17种PAEs在0.5~200 μg/L范围内线性良好,相关系数均大于0.99;PAHs方法检出限为0.6~1.0 μg/kg,方法定量限为1.9~3.3 μg/kg,阴性样品3个添加水平的平均回收率为86.4%~112.2%;PAEs方法检出限为0.4~2.3 μg/kg,方法定量限为1.5~7.6 μg/kg,阴性样品3个添加水平的平均回收率为82.2%~114.1%;相对标准偏差均小于10% (n=6)。 A sensitive method for the simultaneous determination of 16 polycyclic aromatic hydrocarbons (PAHs) and 17 phthalic acid esters (PAEs) in cosmetics by gas chromatography-mass spectrometry (GC-MS) coupled with solid-phase extraction (SPE) was established.Samples were ultrasonically extracted with acetonitrile,purified using PSA/Slica Glass SPE column,separated using Agilent Select PAH chromatographic column and detected by GC-MS with selected ion monitoring (SIM).Results indicate that the linear relationship of 16 PAHs and 17 PAEs in the range of 0.5-200 μg/L is good,with correlation coefficient greater than 0.99.The limits of detection and quantification of the method for PAHs are in the range of 0.6-1.0 and 1.9-3.3 μg/kg,respectively,the average recoveries of negative samples at three spiked levels are between 86.4% and 112.2%.The limits of detection and quantification of the method for PAEs are in the range of 0.4-2.3 and 1.5-7.6 μg/kg,respectively,the average recoveries of negative samples at three spiked levels are between 82.2% and 114.1%,and the relative standard deviation (RSD,n=6) is less than 10%.

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