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2017年, 第47卷, 第5期　刊出日期：2017-05-22 上一期    下一期

基础研究

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烷基磷酸酯与共轭亚油酸形成杂化囊泡的研究 Study on formation of hybrid vesicles with alkyl phosphate and conjugated linoleic acid 梁潇丹, 程若辉, 方云, 樊晔, 张豪杰, 何怡静 2017 (5):  241-245.  doi: 10.13218/j.cnki.csdc.2017.05.001 摘要 ( 273 )   PDF(3684KB) ( 349 )   脂肪酸囊泡(FAV)的中空壳核结构能够包埋活性分子。为改善FAV仅在其pKa附近形成的缺陷,以拓宽FAV的应用范围,将安全性和温和性阴离子表面活性剂烷基磷酸酯钾盐(MAPK)添加到共轭亚油酸中,通过动态激光光散射(DLS)和透射电子显微镜(TEM)研究了囊泡化的pH窗口,发现9% MAPK存在时就可以在中性至酸性环境中形成杂化FAV,不明显改变原有FAV的形貌及粒径,且随着MAPK添加量的增大,杂化FAV的pH窗口有逐渐拓宽的趋势。这一结果显示了杂化FAV在化妆品和个人卫生护理用品等领域的应用前景。 Fatty acid vesicles (FAVs) with a hollow core-shell structure can entrap reactive molecules.In order to improve the defect that FAVs can form near its pKa only so as to enlarge their application field,mild anionic surfactant potassium alkyl phosphate (MAPK) was added to conjugated linoleic acid (CLA).The pH window for vesicles formation was characterized by dynamic light scattering (DLS) and transmission electron microscopy (TEM).It was found that hybrid FAVs can be formed at neutral to acidic environment by blending CLA with 9% MAPK without significant change of morphology and particle size of the original FAVs,and the pH window of the hybrid FAVs has a tendency to gradually broaden along with increasing of the dosage of MAPK.The result shows the potential application of FAVs in fields of cosmetics and personal health care products. 参考文献 | 相关文章 | 计量指标

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“干浓硫酸”的制备与性质研究 Preparation and property of “dry concentrated sulfuric acid” 侯屹婷, 关茹群, 郝雅娟, 杨恒权 2017 (5):  246-250.  doi: 10.13218/j.cnki.csdc.2017.05.002 摘要 ( 303 )   PDF(4944KB) ( 339 )   用十三氟辛基三甲氧基硅烷对SiO2纳米球(SN)表面进行功能化修饰,制得了耐腐蚀的超疏水SiO2纳米球(SN-F)。将SN-F与90%浓硫酸在高速搅拌下混合,成功地制备了“干浓硫酸”,即空气包浓硫酸反相气泡。探讨了SN-F用量对形成“干浓硫酸”的影响,当SN-F的用量为浓硫酸质量的5%时,“干浓硫酸”为粒径100～200 μm间均匀的球体。通过此方法制得的“干浓硫酸”形貌均匀、比表面积大,具有一定的机械强度,且其形貌及性质在18个月后没有改变,为浓硫酸的安全运输、储存、化学反应等应用提供了新的机会。 Functional modification of surface of SiO2 nanoparticles (SN) with 1H,1H,2H,2H-perfluoro-octanetrimethoxysilane was conducted,and corrosion resisting super hydrophobic SiO2 nanoparticles (SiN-F) were prepared.Then “dry concentrated sulfuric acid”,which is sulfuric acid encapsulated in air inverse phase bubbles was prepared by mixing SN-F and 90% concentrated sulfuric acid under high speed stirring.The effect of the dosage of SN-F on formation of “dry concentrated sulfuric acid” was examined.Result shows that when the dosage of SN-F is 5% of the mass of concentrated sulfuric acid,morphology of the “dry concentrated sulfuric acid” is uniform spherical with particle size of 100-200 μm.The prepared “dry concentrated sulfuric acid” displays high specific surface area and certain mechanical strength.After 18 months,its morphology and properties remain unchanged.The method provides new opportunities for safety in transportation,storage and chemical reaction operations in industrial applications of concentrated sulfuric acid. 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(Ⅴ)——离子液体表面活性剂的聚集热力学和状态 Synthesis and application of ionic liquid surfactants (Ⅴ)Thermodynamics and behavior of surfactant aggregation 邹文苑, 杨许召, 徐清杰, 王萍, 王军 2017 (5):  251-256.  doi: 10.13218/j.cnki.csdc.2017.05.003 摘要 ( 309 )   PDF(4639KB) ( 390 )   离子液体表面活性剂聚集形成胶束的ΔG0、ΔH0和ΔS0数据表明,聚集过程为熵驱动;离子液体表面活性剂的聚集数与传统表面活性剂相似,一般在40~160之间,其表观流体力学直径(Dh)为数纳米,高浓度形成囊泡时Dh可达100 nm;胶束表面反离子电离度在0.15~0.6之间;离子液体表面活性剂在水和有机溶剂中的聚集状态有差异,在水中的聚集状态与传统表面活性剂相似。 Aggregation of ionic liquid surfactants in aqueous solution is an entropy driven process,according to the data of its ΔG0,ΔH0 and ΔS0.Aggregation number of ionic liquid surfactants is similar to that of traditional surfactants,40-160 in general.The apparent hydrodynamic diameter (Dh) of surfactant aggregation is several nanometers;but in case the concentration of the ionic liquid surfactant is high as forming vesicles,Dh may achieve 100 nm.Ionization degree of counter ions at the surface of surfactant micelles is about 0.15-0.6.Aggregation behavior of ionic liquid surfactants in water is similar to that of traditional surfactant,but the aggregation behavior of ionic liquid surfactants in water is different with that in organic solvents. 参考文献 | 相关文章 | 计量指标

开发与应用

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剑麻皂苷的萃取与絮凝工艺优化研究 Enrichment of sisal saponin from sisal waste liquor by surfactant solution extraction and flocculation 李祥, 蔺旺梅, 李华锋, 黄尚顺 2017 (5):  257-262.  doi: 10.13218/j.cnki.csdc.2017.05.004 摘要 ( 297 )   PDF(787KB) ( 324 )   以剑麻膏为原料,考察了表面活性剂的种类及浓度、料液比、超声功率、萃取时间、萃取次数和浸泡时间对剑麻皂苷萃取的影响。确定较佳萃取条件为:十二烷基硫酸钠浓度0.025 8 mol/L,料液比1∶10 (g∶mL),超声功率120 W,萃取时间40 min,萃取次数3次,浸泡时间4 h。同时考察了絮凝剂的种类及添加量、絮凝温度和复合絮凝剂对剑麻皂苷富集的影响。确定较佳絮凝条件为:100 mL剑麻皂苷萃取液中先加20 mL 1%聚合氯化铝,再加2 mL 0.1%阳离子聚丙烯酰胺的复合絮凝剂,絮凝温度50 ℃。对在较佳的萃取和絮凝条件下所得絮凝物进行水解,结果显示,该工艺得到的剑麻皂素的质量比传统工艺提高了15.5%,每生产1 g剑麻皂素酸用量减少了81.2%,COD排放量减少了96.5%。 In the process for preparation of sisal fiber,waste liquor that containing sisal saponin is by-produced.In order to make use of the saponin,enrichment process is to be performed.Traditional enrichment process was based upon extraction with an organic solvent.A new approach using a surfactant was tested via a series of experiment.Suitable process conditions were obtained as follows:extracting agent,sodium lauryl sulfate with concentration of 0.025 8 mol/L;ratio of starting material to extracting agent,1∶10 (g∶mL);pre-soaking time,4 h;ultrasonic power,120 W;extraction time,40 min for three times.The extract was further processed for enrichment of the sisal saponin in 100 mL extract under conditions as:temperature,50 ℃;adding 20 mL of 1% aluminum chloride polymer,followed by adding 2 mL of 0.1% cationic polyacrylamide.Under the above mentioned conditions of extraction and flocculation,the flocculated material was hydrolyzed by sulfuric acid.Results show that as comparing with the traditional process,the new approach can increase the product yield for 15.5%,decrease 81.2% of acid consumption and 96.5% of COD discharge per 1 g sisal saponin. 参考文献 | 相关文章 | 计量指标

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蛋白污布的染制均匀性对洗涤剂去污力评价的影响 Effect of dying uniformity of protein stained swatch on detergency evaluation 郭海燕, 姚晨之, 严方, 沈俊 2017 (5):  263-266.  doi: 10.13218/j.cnki.csdc.2017.05.005 摘要 ( 308 )   PDF(712KB) ( 398 )   采用球磨机代替手工磨制炭黑制备改进蛋白污布(改进JB-02),通过测试标准洗衣粉、市售洗衣粉和含蛋白酶的标准洗衣粉对改进JB-02的去污值来评价所制备污布的质量。结果表明,使用球磨机磨制相比于手工磨制的炭黑颗粒的粒径变小,粒度分布变窄,分散均匀性提高;改进JB-02的染制均一度提高;标准洗衣粉对改进JB-02的去污值提高;当标准洗衣粉中蛋白酶的质量分数低于0.15%时,改进JB-02对蛋白酶的敏感度提高;改进JB-02的稳定性较好,可考虑作为标准产品使用。 The preparation method of improved protein stained swatch (Improved JB-02) using ball mill instead of hand grinding was studied,and the quality of the Improved JB-02 was evaluated by comparison of the detergency value of standard laundry powder,market commodity laundry powder and standard laundry powder containing alkaline protease.Results show that after using the ball mill,the carbon black particle size is smaller,the particle size distribution is narrower,the dispersion uniformity is improved,and the dying levelling property of the stained swatch is improved.Furthermore,the detergency value of the standard laundry powder sample formulated with protease mass fraction lower than 0.15% becomes higher since the use of Improved JB-02.It indicates that the Improved JB-02 is more sensitive to protease and displays good storage stability.It can be considered as a standard tool for the evaluation of detergency of laundry products. 参考文献 | 相关文章 | 计量指标

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一种基于聚丙烯酰胺阳离子复合絮凝剂的制备研究 Preparation of a composited cationic flocculant based on polyacrylamide 林福华, 刘功飞 2017 (5):  267-271.  doi: 10.13218/j.cnki.csdc.2017.05.006 摘要 ( 242 )   PDF(726KB) ( 368 )   采用二甲基二烯丙基氯化铵(DMDAAC)对由丙烯酰胺(AM)、微晶纤维素(MCC)和凹凸棒土组成的复合絮凝剂在引发剂偶氮二异丁基咪二盐酸盐作用下进行原位改性,制备出一种新型絮凝剂PDAC。考察了不同反应条件得到的样品对高岭土模拟浊度水的浊度去除率的影响,结果表明,以AM的质量为基准,当体系初始固含量为20%,DMDAAC用量为40%,引发剂用量为0.3%,酸活化凹凸棒土用量为60%,MCC用量为80%,反应温度为60 ℃,反应时间为7 h时,PDAC的絮凝性能较佳,对高岭土模拟浊度水的浊度去除率为96.37%,该数据明显优于不添加DMDAAC的样品。对样品稳定性的测试表明,加入DMDAAC后,PDAC的储存稳定性有了一定程度的提高。 A new type composite flocculant PDAC was prepared by in-situ modification of blend composed of acrylamide (AM),microcrystalline cellulose (MCC) and attapulgite by dimethyldiallylammonium chloride (DMDAAC) with 2,2′-azo bis[2-methylpropionamidine] dihydrochloride as initiator.Effects of different reaction conditions on turbidity removal result were examined with artificial prepared kaolin-water suspension as the simulated turbid water for testing.Results show that with the mass of AM as the standard basis,when the initial solid dosage is 20%,the DMDAAC dosage is 40%,the dosage of initiator is 0.3%,acid the activated attapulgite dosage is 60%,MCC is 80%,the reaction temperature is 60 ℃,and the reaction time is 7 h,the flocculation performance of PDAC is better and the turbidity removal rate achieves 96.37%,which is better than that of sample without use of DMDAAC.Further,stability test result shows that the storage stability of PDAC is improved to some extent after the addition of DMDAAC. 参考文献 | 相关文章 | 计量指标

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广藿香精油抗炎祛痘功效研究 Anti-acne efficacy of essential oil from Pogostemon cablin (Blanco) Benth. 王玥, 郭苗苗, 施雁勤, 潘仙华, 卢艳花, 曹平 2017 (5):  272-276.  doi: 10.13218/j.cnki.csdc.2017.05.007 摘要 ( 484 )   PDF(783KB) ( 394 )   采用气相色谱-质谱联用技术对广藿香精油成分进行分析。通过细胞毒性实验确定广藿香精油对人急性单核细胞(THP-1)的安全质量浓度。利用痤疮丙酸杆菌(P.acnes)刺激THP-1建立的特异性痤疮炎症细胞模型考察广藿香精油对炎症因子IL-1β的影响。通过荧光实时定量逆转录聚合酶链反应(qRT-PCR)初步探讨广藿香精油抗炎祛痘的作用机制。研究结果表明:广藿香精油在最大安全质量浓度12.5 mg/L时,对炎症细胞模型中P.acnes活性影响较小,对IL-1β的分泌具有明显的抑制作用(抑制率66.54%),可显著降低细胞内Toll样受体2(TLR2) mRNA的转录(抑制率73.73%),从而起到抑制炎症信号转导和继发性炎症介质生成的作用。 Chemical composition of the essential oil from Pogostemon cablin (Blanco) Benth.(EOP) was quantitatively analyzed by gas chromatography-mass spectrometry (GC-MS).The safe mass concentration of the EOP to Human Acute Mononuclear Cells (THP-1) was determined via cytotoxicity screening test.An inflammatory acne model was established by stimulating THP-1 with Propionibacterium acnes (P.acnes).Subsequently,the effect of the EOP on the expression of proinflammatory cytokine IL-1β was assessed.The anti-acne mechanism of the EOP was examined by qRT-PCR.Results show that at maximum safe mass concentration of 12.5 mg/L of the EOP,the influence on the activity of P.acnes is rather small and the secretion of IL-1β is significantly inhibited by a rate of 66.54%.The EOP also significantly reduces the mRNA level of Toll-like receptor 2 (TLR2) by 73.73%.Thereby,the EOP inhibits proinflammatory signal transduction and production of secondary inflammatory mediators. 参考文献 | 相关文章 | 计量指标

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苯乙醇微胶囊的稳定性及热释放行为研究 Study on stability of phenethyl alcohol microcapsules and their thermal releasing behavior 沈靖轩, 肖维毅, 徐兰兰, 刘哲, 沈妍, 黄海群 2017 (5):  277-280.  doi: 10.13218/j.cnki.csdc.2017.05.008 摘要 ( 345 )   PDF(5439KB) ( 306 )   以苯乙醇为囊芯材料,以明胶和羧甲基纤维素(CMC)为壁材,采用复凝聚法制备了苯乙醇微胶囊,其包埋率达到92%。考察了温度和时间对苯乙醇微胶囊热释放行为的影响,以及其在卷烟纸上的贮存稳定性。结果表明,苯乙醇微胶囊可粘附在纸张纤维上,120 ℃加热10 min时微胶囊基本无变化,能够满足卷烟纸生产工艺要求。180 ℃加热40 min时微胶囊内部芯材基本挥发完全。在常温下密封保存60 d时苯乙醇保留率仍达到65%,稳定性较好。 Phenethyl alcohol microcapsules were prepared by complex coagulation method with phenethyl alcohol as core material as well as gelatin and carboxyl methyl cellulose as wall materials.The microcapsule embedding rate achieves 92%.Effects of temperature and time on thermal releasing behavior of the phenethyl alcohol microcapsules as well as their storing stability on cigarette paper were examined.Results show that the phenethyl alcohol microcapsules can adhere on the paper fibers,and basically maintain no change at 120 ℃ for 10 min;so it can satisfy the main technological requirement for the cigarette paper.Basically,the core material of the microcapsules can volatilize completely at 180 ℃ for 40 min;while after storing under close and room temperature for 60 d,the retention rate of micro-capsulated phenethyl alcohol reaches 65%.It shows that the storing stability of the microcapsules is good. 参考文献 | 相关文章 | 计量指标

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H6P2Mo9W9O62/Cu3(BTC)2的制备及催化合成缩醛(酮) Preparation of H6P2Mo9W9O62/Cu3(BTC)2 and its catalytic performance for synthesis of acetals and ketals 向诗银, 杨水金 2017 (5):  281-285.  doi: 10.13218/j.cnki.csdc.2017.05.009 摘要 ( 217 )   PDF(1578KB) ( 310 )   采用浸渍法制得H6P2Mo9W9O62/Cu3(BTC)2,利用傅里叶变换红外光谱仪(FT-IR)、X射线衍射仪(XRD)、热重分析仪(TG)以及扫描电镜(SEM)表征其组成、结构、热稳定性以及形貌。以H6P2Mo9W9O62/Cu3(BTC)2为催化剂,环己酮和乙二醇合成缩酮的反应为探针,探究出较佳反应条件:环己酮用量为0.2 mol,n(环己酮)∶n(乙二醇)=1∶1.3,催化剂用量占反应物总质量的0.3%,反应时间为60 min,带水剂用量为6 mL。在此条件下,环己酮乙二醇缩酮收率可达83.7%。且以上条件下催化合成苯甲醛乙二醇缩醛、丁酮乙二醇缩酮、丁酮1,2-丙二醇缩酮、苯甲醛1,2-丙二醇缩醛和环己酮1,2-丙二醇缩酮的收率分别为70.1%,66.0%,62.1%,66.3%和75.8%。与分子筛MCM-48负载硅钨酸、活性炭负载对甲苯磺酸和铝交联蒙脱土催化剂相比,H6P2Mo9W9O62/Cu3(BTC)2是一种催化性能较好的催化剂。 H6P2Mo9W9O62/Cu3(BTC)2 as a new catalyst was prepared by impregnation method.Fourier transformation infrared spectrum (FT-IR),X-ray diffraction (XRD),thermal gravimetry (TG) and scanning electron microscope (SEM) were used for characterization and measurement of its composition,structure,thermal stability and morphology.The reaction,with H6P2Mo9W9O62/Cu3(BTC)2 as catalyst,for synthesis of ketal from cyclohexanone and ethylene glycol as starting materials was used as probe reaction,and the optimized synthesis conditions were found by orthogonal experiments as follows:fixing the amount of cyclohexanone as 0.2 mol;molar ratio,n(cyclohexanone)∶n(ethylene glycol)=1∶1.3;mass ratio of the catalyst to total reactants,0.3%;the reaction time,60 min;and amount of water stripping agent,6 mL.The yield of the product reaches 83.7%.Under similar reaction conditions,the yield of benzaldehyde ethylene glycol acetal reaches 70.1%;butanone glycol ketal,66.0%;butanone 1,2-propylene glycol ketal,62.1%;benzaldehyde 1,2-propanediol acetal,66.3%;and cyclohexanone 1,2-propylene glycol ketal,75.8%.Compared with that of catalysts H4SiW12O40/MCM-48,activated carbon supported p-toluene sulfonic acid and Al-cross linked montmorillonite,H6P2Mo9W9O62/Cu3(BTC)2 shows better catalytic performance. 参考文献 | 相关文章 | 计量指标

专论与综述

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头发光损伤评价方法 A review of the evaluation methods for hair photodamage 曹月, 瞿昊 2017 (5):  286-291.  doi: 10.13218/j.cnki.csdc.2017.05.010 摘要 ( 386 )   PDF(5299KB) ( 484 )   对头发光损伤及表现进行了简单介绍,对评价头发光损伤形貌变化以及化学物质变化的方法进行了详细综述,重点介绍了多光谱成像技术及其在头发光损伤评价中的应用。 Phenomenon of human hair photodamage was briefed.The methods for evaluating the changes in morphology and chemical materials of human hair were reviewed in detail.Finally,the multi-spectral imaging technology and its application in the evaluation of hair photodamage were introduced emphatically. 参考文献 | 相关文章 | 计量指标

分析与检测

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气相色谱-质谱联用法测定膏霜类化妆品中10种合成麝香 Determination of ten kinds of synthetic musk in cream cosmetics by GC-MS 宁啸骏, 周静, 符昌雨 2017 (5):  292-296.  doi: 10.13218/j.cnki.csdc.2017.05.011 摘要 ( 264 )   PDF(1550KB) ( 372 )   建立了膏霜类化妆品中10种合成麝香的气相色谱-质谱联用(GC-MS)分析方法。样品加入氘代同位素内标后,用正己烷提取,提取液经基体分散固相萃取(MSPD)净化处理,以VF-WAXms毛细管色谱柱分离,选择特征离子监测(SIM)扫描模式测定,采用标准曲线法定量。结果表明,10种合成麝香的线性范围为0.01～0.2 mg/L,相关系数均大于0.99,定量限为0.05～0.10 mg/kg,加标回收率为80.1%～102.2%,相对标准偏差(RSD)均小于5%。 An analytical method was established for simultaneous determination of ten kinds of synthetic musk in cream cosmetics using gas chromatography-mass spectrometry (GC-MS).Samples were spiked with deuterium-labeled isotope internal standards and extracted by n-hexane.Then the extract was purified with matrix solid-phase dispersion (MSPD) and separated by a VF-WAXms capillary column.All the compounds were detected with selected ion monitoring (SIM) scanning mode.Quantification was carried out using standard plot calibration.Results show that the ten kinds of synthetic musk display a good linear relationship within the mass concentration range of 0.01-0.2 mg/L and the correlation coefficients are all higher than 0.99.The quantification limits (LOQs) of the synthetic musk are in the range of 0.05-0.10 mg/kg.Values of spiked recoveries are found to be from 80.1% to 102.2% with all relative standard deviations (RSD) lower than 5%. 参考文献 | 相关文章 | 计量指标

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超高效液相色谱-串联质谱法测定染发剂中9种染料 Simultaneous determination of nine kinds of dyestuff in hair dyes by ultra performance liquid chromatography-tandem mass spectrometry 戴明 2017 (5):  297-300.  doi: 10.13218/j.cnki.csdc.2017.05.012 摘要 ( 253 )   PDF(714KB) ( 392 )   建立了同时测定染发剂中9种染料的超高效液相色谱-串联质谱分析方法。样品用甲醇进行超声提取,以10 mmol/L 乙酸铵水溶液-乙腈为流动相,BEH-C18色谱柱(2.1 mm×100 mm,1.7 μm)分离待测物,采用电喷雾离子源,正离子扫描和多反应监测(MRM)模式检测,外标法进行定量。9种染料羟乙基-2-硝基-p-甲苯胺、4-羟丙氨基-2-硝基苯酚、4-氨基-N,N-二甲基苯胺、3-硝基-p-羟乙氨基苯酚、2,6-二羟乙氨基甲苯、2-甲基-5-羟乙氨基苯酚、5-氨基-6-氯-2-甲基苯酚、2,6-二甲氧基-3,5-吡啶二胺盐酸盐和6-氨基间甲酚的检出限分别为1.7,0.84,0.27,3.4,0.034,1.2,7.0,0.17和0.20 mg/kg。样品加标回收实验的平均加标回收率为90.0%~110.0%,相对标准偏差为1.4%~8.6%(n=6)。该方法快速简便,定量准确,能够满足染发剂中染料含量的分析检测要求。 A method for simultaneous determination of nine kinds of dyestuff in hair dyes by UPLC-MS/MS was established.The hair dye sample was extracted by methanol under assistance of ultrasonic irradiation.The separation was performed by a BEH-C18 column (2.1 mm×100 mm,1.7 μm) with gradient elution of 10 mmol/L ammonium acetate and acetonitrile as mobile phase.The electrospray ionization (ESI) source with positive ion mode was used for the analysis of the nine components in the multiple reaction monitoring (MRM) mode.External standard method was used for quantification.The limit of detection of the nine kinds of dyestuff,including 2-(4-methyl-2-nitrophenylamino) ethanol,3-nitro-N-(2-hydroxyethyl)-4-aminophenol,4-amino-N,N-dimethylaniline,4-((2-hydroxypropyl) amino)-2-nitrophenol,bis-2,6-N,N-(2-hydroxyethyl) diaminotoluene,5-((2-hydroxyethyl) amino)-o-cresol,5-amino-6-chloro-2-methylphenol,3,5-diamino-2,6-dimethoxypyridine dihydrochloride and 6-amino-m-cresol are 1.7,0.84,0.27,3.4,0.034,1.2,7.0,0.17 and 0.20 mg/kg,respectively.The average recoveries of the nine kinds of dyestuff in the spiked samples are in the range of 90.0%-110.0% with the relative standard deviations (RSD,n=6) of 1.4%-8.6%.This method is simple,accurate and effective for simultaneous determination of the nine kinds of dyestuff in hair dyes. 参考文献 | 相关文章 | 计量指标