当期目录

2014年, 第44卷, 第12期　刊出日期：2014-12-22 上一期    下一期

基础研究

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Bola型非对称阳离子表面活性剂的合成及性能研究 Synthesis and performance of Bolaform asymmetrical cationic surfactants 王军, 陈翔, 杨许召, 宋浩, 邹文苑, 陈玉菲 2014 (12):  661-665.  doi: 10.13218/j.cnki.csdc.2014.12.147 摘要 ( 279 )   PDF(945KB) ( 390 )   以α,ω-二溴代烷、丁基咪唑和三丁基膦为原料经过二步反应合成了3种Bola型非对称阳离子表面活性剂。中间体1-(12-溴十二烷基)-3-丁基咪唑溴盐的较佳合成工艺条件为:n(丁基咪唑):n(1,12-二溴十二烷):n(四丁基碘化铵)=1:1.5:0.005,异丙醇作溶剂,反应温度65 ℃,反应时间6 h;Bola型表面活性剂的合成工艺条件为:n(1-(12-溴十二烷基)-3-丁基咪唑溴盐):n(三丁基膦)=1.05:1,微波辅助反应,反应温度80 ℃,反应时间12 h。所合成的Bola型表面活性剂表现出了优良的表面活性,30 ℃时cmc在5.7×10-3~8.7×10-2 mol·L-1之间、γcmc在30~36 mN·m-1之间;随着碳链长度的增长,其cmc,γcmc及分子最小横截面积(Amin)逐渐减小,饱和吸附量(Γmax)和吸附效率(pc20)逐渐增大。 Three kinds of Bolaform asymmetrical cationic surfactant were synthesized through two step reaction with α,ω-dibromo alkane,n-butyl imidazole and tributylphosphine as starting materials.Optimized conditions for preparation of the intermediate 1-(12-bromo-dodecyl)-3-butylimidazolium bromide are:n(n-butyl imidazole):n(1,12-dibromo-dodecane):n(tetrabutylammonium iodide)=1:1.5:0.005;at 65 ℃ for 6 h with isopropanol as solvent.Conditions for preparation of the product are:n(1-(12-bromo-dodecyl)-3-butylimidazolium bromide):n(tributylphosphine)=1.05:1;at 80 ℃ for 12 h with assistance of microwave irradiation.The synthesized products display good surface active performance.Their cmc is 5.7×10-3~8.7×10-2 mol·L-1;γcmc is 30~36 mN·m-1 at 30 ℃.With increasing of the carbon chain length,their cmc,γcmc and Amin decreases,while Γmax and pc20 increases. 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(Ⅻ) ——表面活性剂的分散作用及其应用 Performance and applications of surfactants (Ⅻ) Dispersing function of surfactants and its applications 王楠, 张桂菊, 赵莉, 徐宝财 2014 (12):  666-670.  doi: 10.13218/j.cnki.csdc.2014.12.148 摘要 ( 362 )   PDF(817KB) ( 592 )   综述了表面活性剂的分散作用及其应用领域,重点介绍了表面活性剂在钙皂分散、颜料分散、纳米粒子分散、农药及其他方面的分散作用原理及应用研究进展,并对表面活性剂作为分散剂的应用前景进行了展望。 Dispersing function of surfactants and its applications were reviewed.Progress in the research work with respect to mechanism and applications in lime soap dispersion,pigment dispersion,nano-particles dispersion,pesticides and other aspects were focused.The future development about application of surfactants as dispersant was prospected. 参考文献 | 相关文章 | 计量指标

开发与应用

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三元复合体系色谱分离实验研究 Experimental study on chromatographic separation phenomenon of ternary composite oil displacement agent system 刘凯, 岳湘安, 杨长春, 苏群, 徐金涛, 张德鑫 2014 (12):  671-675.  doi: 10.13218/j.cnki.csdc.2014.12.149 摘要 ( 295 )   PDF(848KB) ( 386 )   利用填砂管模型进行了三元复合体系的渗流实验,研究了填砂管渗透率及长度对于三元复合体系色谱分离的影响。实验结果表明,在填砂管渗透率和长度不同的条件下,三元复合体系均发生了明显的色谱分离现象。当填砂管渗透率从0.601 μm2减小到0.390 μm2时,三元复合体系色谱分离程度增加;当填砂管长度从100 cm增加到240 cm时,三元复合体系色谱分离程度有所增加。说明填砂管渗透率和长度是影响三元复合体系色谱分离的重要因素,且填砂管渗透率的变化对于三元复合体系色谱分离影响程度大于长度。 Seepage flow test of alkali-surfactant-polymer ternary composite oil displacement agent system (hereinafter refers to as the ASP system) was conducted with Sandpack model.Effect of permeability and length of the Sandpack on chromatographic separation phenomenon of the ASP system was investigated.Experimental results showed that under all separate conditions of permeability and length of the Sandpack,the ASP system displays remarkable chromatographic separation phenomenon.When the permeability reduces from 0.601 μm2 to 0.390 μm2,the extent of chromatographic separation increases while when the length of the Sandpack increases from 100 cm to 240 cm,the extent of chromatographic separation displays somewhat increment.Such results indicated that both permeability and length of the Sandpack affect the chromatographic separation of the ASP system;while effect of the permeability is stronger than that of the length. 参考文献 | 相关文章 | 计量指标

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4A分子筛的水热法合成工艺研究 Investigation of synthesis conditions of 4A zeolite with hydro-thermal method 卢传竹, 赵华, 李会鹏, 赵晓隆, 李智超 2014 (12):  676-679.  doi: 10.13218/j.cnki.csdc.2014.12.150 摘要 ( 352 )   PDF(1027KB) ( 453 )   采用水热法合成了4A分子筛,以4A分子筛的钙离子交换度为指标,通过单因素试验和正交试验考察了4A分子筛的合成条件。实验结果表明,合成4A分子筛的最佳条件为:n(SiO2)/n(Al2O3)=1.8,n(Na2O)/n(SiO2)=3.0,n(H2O)/n(Na2O)=40,晶化温度为100 ℃(常压),晶化时间为6 h。在此条件下合成的4A分子筛的钙离子交换度为323 mg·g-1。同时通过XRD和SEM对最佳条件下的4A分子筛进行了表征。 4A zeolite was synthesized with hydro-thermal method.The synthesis conditions were investigated via single factor experiment and orthogonally designed experiment using the calcium ion exchange capacity of 4A zeolite as index.The optimal reaction conditions were determined as:n(SiO2)/n(Al2O3)=1.8;n(Na2O)/n(SiO2)=3.0;n(H2O)/n(Na2O)=40;crystallization temperature of 100 ℃ (normal pressure) and crystallization time of 6 h.Calcium ion exchange capacity of the product achieves 323 mg·g-1.The product was characterized by XRD and SEM. 参考文献 | 相关文章 | 计量指标

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金莲花挥发性组分色谱保留值的构效关系研究 Study on quantitative structure-retention relationship of volatile components in Trollius chinensis Bunge 秦文斌, 冷检, 秦正龙, 冯长君 2014 (12):  680-682.  doi: 10.13218/j.cnki.csdc.2014.12.151 摘要 ( 217 )   PDF(754KB) ( 414 )   为了研究金莲花挥发性组分的色谱保留性质,基于分子价连接性指数(mXtV)和原子类型电性拓扑状态指数(Ek),构建金莲花挥发性组分分子结构与色谱保留时间的定量构效关系模型,其多元线性回归方程的相关系数为0.987,并用Jackknife法对模型的稳健性进行检验,其相关系数均在0.985～0.989之间,具有高度的稳健性和良好的预测能力,有效地揭示了影响金莲花挥发性组分色谱保留时间的本质因素。 In order to study chromatographic retention time of volatile components in Trollius chinensis Bunge,molecular valence connectivity index (mXtV) and atom-type electro-topological state index (Ek),were used to characterize the structures of 38 volatile compounds from Trollius chinensis Bunge.The quantitative structure-retention relationship model using mXtV and Ek was developed to predict chromatographic retention time of volatile components in Trollius chinensis Bunge.The correlation coefficient (R) of the model is 0.987.The robustness of the regression model was validated by Jackknife method,and the results showed that the R lies between 0.985 and 0.989.The present study demonstrates that the model is highly reliable and has favorable predictive capacity,and can effectively elucidate the essential factor that affecting the chromatographic retention time of volatile compounds in Trollius chinensis Bunge. 参考文献 | 相关文章 | 计量指标

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可用于化妆品中水溶性丝胶粉的性能研究 Properties of water soluble sericin powder used in cosmetics 孙道权, 庄愉, 盛家镛, 邢铁玲, 陈国强, 徐婕 2014 (12):  683-687.  doi: 10.13218/j.cnki.csdc.2014.12.152 摘要 ( 256 )   PDF(998KB) ( 450 )   将蚕丝脱胶后的丝胶溶液经过脱色、酶解、离子交换纯化、浓缩、喷雾干燥等加工得到水溶性丝胶粉。对制得的丝胶粉进行了氨基酸组分分析和分子质量测定,并对其进行了抑制酪氨酸酶活性及对皮肤的保湿和吸湿性能考察。结果表明:丝胶粉中主要含有16种氨基酸;丝胶粉分子质量大小不同其应用体系亦不同;丝胶粉质量分数为1%时对皮肤黑色素生成的抑制率可达52.39%;电镜观察显示丝胶粉对头发有很好的护理和修复效果。 Water soluble sericin powder product was prepared with sericin solutions obtained from degumming of silk by processing including decolorization,enzymatic hydrolysis,ion exchange purification,concentration,and spray drying et al.Amino acid composition analysis,molecular mass determination,inhibition effect of tyrosinase activity,skin moisturizing as well as hygroscopic performance of the sericin powder product were investigated.Results showed that,the sericin powder product mainly contains 16 kinds of amino acid;sericin powder products with separate molecular mass were suitable for different application fields;when mass fraction of the sericin powder product is 1%,the inhibition ratio on skin melanin achieves 52.39%.Electron microscope observation showed that the sericin powder product displays good nursing and restoring effect on human hair. 参考文献 | 相关文章 | 计量指标

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曲酸金属配合物的合成与酪氨酸酶抑制性能研究 Synthesis and tyrosinase inhibitory activity of kojic acid metal complexes 杨培, 张逸伟 2014 (12):  688-691.  doi: 10.13218/j.cnki.csdc.2014.12.153 摘要 ( 252 )   PDF(862KB) ( 521 )   曲酸(KA)与4种金属离子配位反应得到相应的曲酸金属配合物KA-Fe(Ⅲ),KA-Cu(Ⅱ),KA-Mn(Ⅱ)和KA-Zn(Ⅱ),采用红外光谱、差热-热重分析和紫外光谱对其金属配合物进行了结构表征,并进行了对酪氨酸酶的抑制作用研究。结果表明,KA-Fe(Ⅲ),KA-Zn(Ⅱ)和KA-Mn(Ⅱ)对酪氨酸酶的抑制效果显著,对应的IC50为25,18和62 μmol·L-1(曲酸IC50为70 μmol·L-1),根据抑制机理分析,该系列金属配合物的抑制类型属于非竞争性抑制。 Four kinds of metal complex of kojic acid (KA),KA-Fe(Ⅲ),KA-Cu(Ⅱ),KA-Mn(Ⅱ) and KA-Zn(Ⅱ) were prepared by complexing reaction through kojic acid and metal ion compounds.Their chemical structures were characterized by infrared spectra,differential thermal gravimetric analysis and ultraviolet spectra.Their tyrosinase inhibitory action was examined.Results showed that the tyrosinase inhibitory effect of KA-Fe(Ⅲ),KA-Zn(Ⅱ) and KA-Mn(Ⅱ) are remarkable.Their corresponding IC50 is 25,18 and 62 μmol·L-1 respectively (while IC50 of kojic acid is 70 μmol·L-1).Based upon analysis of their inhibitory mechanism,the type of inhibitory action of this series of compound is all considered as non-competitive inhibition. 参考文献 | 相关文章 | 计量指标

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牡丹花水提液清除羟自由基及抑制酪氨酸酶活性的研究 Study on scavenging effect on hydroxyl free radicals and inhibitory effect on tyrosinase of water extracts from peony 陈佳龄, 张凯, 孙永, 龚盛昭 2014 (12):  692-694.  doi: 10.13218/j.cnki.csdc.2014.12.154 摘要 ( 318 )   PDF(954KB) ( 356 )   采用水提法提取牡丹花制得牡丹花水提液,以Fenton反应产生羟自由基,比色法检测牡丹花水提液清除羟自由基的能力,分别以L-酪氨酸和L-多巴为底物,在30 ℃,pH=6.8的磷酸盐缓冲体系中测定牡丹花水提液对酪氨酸酶单酚酶活性和二酚酶活性的抑制效应。实验结果表明,牡丹花水提液可有效清除羟自由基,牡丹花水提液质量浓度为1.00 g·L-1时,自由基清除率达91.67%;牡丹花水提液对酪氨酸酶单酚酶和二酚酶活性均有良好抑制作用,其IC50分别为0.015和0.210 g·L-1。牡丹花水提液对二酚酶的抑制作用表现为非竞争性抑制,米氏常数(Km)为0.4 mmol·L-1。 The water extract from the flowers of peony was prepared.Scavenging effect on hydroxyl free radicals,which were generated from the Fenton reaction of the water extracts was detected by spectrophotometry.The inhibitory action of water extracts from peony on the activity of monophenolase and diphenolase contained in tyrosinase were studied by using L-tyrosine and L-DOPA (L-3,4-dihydroxyphenylalanine) as substrate separately at 30 ℃ with Na2HPO4-NaH2PO4 as buffer solution (pH=6.8).The results showed that the water extracts from peony can scavenge hydroxyl free radicals effectively.The free radical elimination ratio of the water extracts achieves 91.67% when the mass concentration of the peony water extract is 1.00 g·L-1.The water extract from peony displays good inhibitory effect to both monophenolase and diphenolase activity of tyrosinase with IC50 at 0.015 g·L-1 for monophenolase and 0.210 g·L-1 for diphenolase.The inhibition kinetics of the water extracts analyzed by Lineweaver-Burk plots demonstrated a non-competitive inhibitor for diphenolase and the Michaelis constant (Km) was determined to be 0.4 mmol·L-1. 参考文献 | 相关文章 | 计量指标

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超声辐射下酸性离子液体催化合成1,1-二乙酸酯 Synthesis of 1,1-diacetates with acidic ionic liquid as catalyst under ultrasonic irradiation 汤小芳, 刘显明, 周昊, 仇涛涛, 储海蓉, 邢志恒 2014 (12):  695-699.  doi: 10.13218/j.cnki.csdc.2014.12.155 摘要 ( 187 )   PDF(835KB) ( 292 )   室温无溶剂超声辐射下,以功能化酸性离子液体[C3SO3Hnhm][HSO4]为催化剂、芳香醛和乙酸酐为原料合成1,1-二乙酸酯。通过单因素试验优化了反应条件,研究了该离子液体的重复使用性能及催化剂的底物适用性。结果表明,当苯甲醛与乙酸酐的摩尔比为1:2.3,20 ℃超声辐射反应15 min,催化剂用量为苯甲醛物质的量的1%时,收率可达96%以上;[C3SO3Hnhm][HSO4]重复使用5次,其催化活性下降不明显;将[C3SO3Hnhm][HSO4]用于其他芳香醛的催化,收率为84%~98%。 Under conditions of room temperature,solvent-free and ultrasonic irradiation,with an aromatic aldehyde and acetic anhydride as starting materials and functionalized acidic ionic liquid [C3SO3Hnhm][HSO4] as catalyst,1,1-diacetates was synthesized.The optimal reaction conditions were found by single factor experiments.Reusing performance of the catalyst as well as applicability of the substrate were investigated.Results showed that when the molar ratio of benzaldehyde and acetic anhydride is 1:2.3;the reaction temperature is 20 ℃;ultrasonic irradiation applies for 15 min;and the dosage of catalyst is 1% of benzaldehyde;the yield can reach more than 96%.The catalyst [C3SO3Hnhm][HSO4] can be reused for 5 times with no significant declining of the catalytic activity.In case the catalyst [C3SO3Hnhm][HSO4] is used to catalyze the reaction of other aromatic aldehydes,the yield achieves 84%-98%. 参考文献 | 相关文章 | 计量指标

专论与综述

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无机防晒剂 Inorganic sunscreening agents 曹智, 张道军 2014 (12):  700-705.  doi: 10.13218/j.cnki.csdc.2014.12.156 摘要 ( 314 )   PDF(879KB) ( 565 )   对无机防晒剂的防晒机理进行了简要介绍,综述了防晒化妆品中纳米无机防晒剂微粒粒径与紫外屏蔽效果之间的关系以及倍受关注的纳米无机防晒剂的安全性问题,主要集中在纳米TiO2和ZnO微粒经皮肤的渗透性和可能存在的光毒性。 Mechanism of inorganic sunscreen was briefly introduced.Relationship between particle size of inorganic sunscreen nanoparticles in sunscreen cosmetics and their UV shielding effect as well as the safety issue of inorganic sunscreen nanoparticles that was concerning seriously by peoples were summarized and focused on percutaneous penetration of TiO2 and ZnO nanoparticles through human skin and their potential to cause phototoxicity. 参考文献 | 相关文章 | 计量指标

分析与检测

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柑橘精油中呋喃香豆素的超高效液相色谱分析 Determination of furocoumarines in citrus essential oil by ultra-high performance liquid chromatography 茅富燕, 庄伟强, 黄健, 乐之歆, 胡坪 2014 (12):  706-709.  doi: 10.13218/j.cnki.csdc.2014.12.157 摘要 ( 227 )   PDF(852KB) ( 419 )   建立了柑橘类精油中4种呋喃香豆素(异补骨脂素、补骨脂素、5-甲氧基补骨脂素和欧前胡素)的超高效液相色谱(UPLC)分析方法。样品经甲醇稀释定容,高速离心分离后,取上清液进样分析。采用Agilent Zorbax Eclipse Plus C18色谱柱(2.1 mm×50 mm,1.8 μm)分离,以水-乙腈二元流动相梯度洗脱,流速0.3 mL·min-1,检测波长300 nm。4种呋喃香豆素在0.5～100 mg·L-1范围内呈良好线性,相关系数均达到0.999,检出限为1.5～3.0 mg·kg-1 ,平均回收率为97.5%～105.6%,相对标准偏差为0.4%～2.9% (n=3)。采用已建立的方法对25批柑橘类精油样品进行测定,发现1个批次的甜圆柚油中含有5-甲氧基补骨脂素,质量分数为60.5 mg·kg-1 。 An analysis method was established to determine four kinds of furocoumarines (isopsoralen,psoralen,5-methoxy-psoralen and imperatorin) in citrus essential oil by ultra-high performance liquid chromatography (UPLC) with a diode array detector (DAD).The essential oil sample was diluted with methanol.After centrifugal separation,the supernatant was directly analyzed by UPLC.The separation was performed on an Agilent Zorbax Eclipse Plus C18 column (2.1 mm×50 mm,1.8 μm),with water-acetonitrile as the mobile phase in gradient elution mode at a flow rate of 0.3 mL·min-1.The detection wavelength was 300 nm.The results indicated that good linearity is obtained in the mass concentration range of 0.5-100 mg·L-1 with all correlation coefficients of 0.999 for the four kinds of furocoumarines.The detection limits are 1.5-3.0 mg·kg-1 .The recoveries at three spiked levels of four kinds of furocoumarines are ranged within 97.5%-105.6%,with the relative standard deviations of 0.4%-2.9% (n=3).Furthermore,25 batches of citrus essential oil samples were determined using the established method and a batch of grapefruit oil was found containing 60.5 mg·kg-1 of 5-methoxy-psoralen. 参考文献 | 相关文章 | 计量指标

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电感耦合等离子体质谱法同时测定化妆品中12种元素 Simultaneous determination of 12 elements in cosmetics by inductively coupled plasma mass spectrometry 王欣美, 王柯 2014 (12):  710-713.  doi: 10.13218/j.cnki.csdc.2014.12.158 摘要 ( 258 )   PDF(778KB) ( 319 )   建立了同时测定化妆品中铬、锰、镍、铜、锌、砷、硒、镉、锑、锡、汞和铅12种元素含量的测定方法。样品经微波消解,采用电感耦合等离子体质谱法(ICP-MS)同时测定12种元素。结果表明,12种元素线性关系良好(r=0.999 6~1.000 0),方法检出限为0.04~0.43 mg·kg-1,重复性实验的相对标准偏差为1.17%~9.69%,回收率为82.9%~115.1%。该方法简便快速、准确性高、可靠性强,可较好的应用于化妆品的元素测定。 A method for determination of 12 elements:chromium (Cr),manganese (Mn),nickel (Ni),copper (Cu),zinc (Zn),arsenic (As),selenium (Se),cadmium (Cd),stibium (Sb),stannum (Sn),mercury (Hg) and lead (Pb) in cosmetics simultaneously was established.After being pretreated with microwave digestion,the 12 elements in cosmetics were detected by inductively coupled plasma mass spectrometry (ICP-MS).Results indicated that the relationship between the responds and the mass concentration of 12 elements shows good linearity with the value of r between 0.999 6 and 1.000 0.The detection limits of the method are between 0.04 and 0.43 mg·kg-1,and the relative standard deviations (RSD) of the repeatability are between 1.17% and 9.69%.Spiked recoveries of 12 elements are between 82.9% and 115.1%.This method is fast,simple,accurate and reliable,which could be applied for element analysis in cosmetics. 参考文献 | 相关文章 | 计量指标

生产与技术

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喷雾法生产石油磺酸盐技术研究 Technology for production of petroleum sulfonate via spray method 方新湘, 牛春革, 白云, 周华 2014 (12):  714-717.  doi: 10.13218/j.cnki.csdc.2014.12.159 摘要 ( 241 )   PDF(846KB) ( 279 )   介绍了喷雾法生产石油磺酸盐的研究情况。根据石油组分的特点,采用喷雾磺化技术大幅度增加了石油组分与三氧化硫的气液接触面积,使得磺化效率得到了很大的提高,磺化反应接触时间从几小时缩短到几十秒,减少了石油组分过磺化现象的发生,小试研究结果表明,与传统釜式磺化技术相比,采用改造后的喷雾磺化工艺使得石油磺酸盐的收率提高了3%以上,酸性油收率提高10%以上,酸渣收率降低35%以上,可实现连续化生产,并为工业化应用提供参考。 Technology for production of petroleum sulfonate via spray method was introduced.Based upon the characteristics of the petroleum fraction,the adoption of spray sulfonation technology increases the contacting surface area between the petroleum fraction and SO3 substantially and results in a great improvement of the sulfonation efficiency.Contacting time for sulfonation reduces from several hours to several ten seconds and thus reduces the happening of over-sulfonation.Results of laboratory tests showed that as comparing with the conventional reaction kettle sulfonation,the spray sulfonation causes more than 3% increase of yield of the petroleum sulfonate and more than 10% increase of yield of the raffinate oil;while the yield of the acid residue decreases for more than 35%.Continuous process can be realized and the laboratory test results can be used as reference for industrial operation. 参考文献 | 相关文章 | 计量指标