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2016年, 第46卷, 第9期　刊出日期：2016-09-22 上一期    下一期

基础研究

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羟乙基纤维素接枝环氧大豆油高分子表面活性剂的合成及性能 Synthesis and performance of polymeric surfactants based on epoxidized soybean oil grafted hydroxyethyl cellulose 黄旭娟,刘鹤,商士斌,沈明贵,蔡照胜 2016 (9):  489-493.  doi: 10.13218/j.cnki.csdc.2016.09.001 摘要 ( 344 )   PDF(990KB) ( 356 )   以羟乙基纤维素(HEC)与环氧大豆油(ESO)为原料,四氯化锡(SnCl4)为催化剂,二甲亚砜(DMSO)为溶剂,在室温下反应制备了羟乙基纤维素接枝环氧大豆油(ESO-HEC);ESO-HEC经碱性水解后,用酸处理得到羟乙基纤维素接枝环氧大豆油水解的酸性产物(H-ESO-HEC);再通过NaOH中和H-ESO-HEC结构中的羧酸基团,得到3种H-ESO-HEC-Na高分子表面活性剂。通过FT-IR表征了3种表面活性剂酸性产物H-ESO-HEC的结构;热重测试表明H-ESO-HEC比HEC具有更好的热稳定性;动态表面张力测试表明当H-ESO-HEC-Na的质量浓度升高,动态表面张力下降,且质量浓度达到临界胶束浓度时,最小表面张力值可达29 mN/m;泡沫性能测试表明随着ESO接枝量的增多,H-ESO-HEC-Na高分子表面活性剂的起泡和稳泡能力逐渐增强;通过对H-ESO-HEC-Na水溶液/庚烷的界面张力进行测试,发现不同条件制备得到的H-ESO-HEC-Na水溶液/庚烷的最低界面张力值接近,为9.8 mN/m左右。 Epoxidized soybean oil grafted hydroxyethyl cellulose (ESO-HEC) was synthesized through the grafting reaction between epoxidized soybean oil (ESO) and hydroxyethyl cellulose (HEC) with stannic chloride (SnCl4) as catalyst in dimethyl sulfoxide (DMSO) as process agent.After hydrolysis in the presence of sodium hydroxide,and the hydrolyzed product was treated with hydrochloric acid,the ESO-HEC converted into an acidic product H-ESO-HEC.Then three kinds of polymeric surfactant,H-ESO-HEC-Na,were obtained through neutralizing the carboxyl groups of H-ESO-HEC.Chemical structure of H-ESO-HEC was characterized by Fourier transform infrared spectroscopy (FT-IR).Thermogravimetric (TG) analysis demonstrated that the thermo-stability of H-ESO-HEC was noticeably higher than that of HEC.The dynamic surface tension of the surfactant decreases as the mass concentration of surfactant increases.Furthermore,when the mass concentration of the surfactant reaches its critical micelle concentration value,the minimum surface tension could reach to 29 mN/m.The results showed that the foaming power and foam stability of the surfactants increases with the increase of ESO that was grafted on HEC.The H-ESO-HEC-Na surfactants prepared under different conditions may reduce heptane/water interfacial tension to a similar value around 9.8 mN/m. 参考文献 | 相关文章 | 计量指标

科技讲座

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氟表面活性剂和氟聚合物(Ⅸ)——全氟磺酸树脂和全氟磺酸离子交换膜 Fluorinated surfactants and fluoropolymers (Ⅸ) Perfluorosulfonic acid resin and perfluorosulfonate ion-exchanged membrane 窦增培,白富栋,邢航,肖进新 2016 (9):  494-501.  doi: 10.13218/j.cnki.csdc.2016.09.002 摘要 ( 484 )   PDF(998KB) ( 688 )   全氟磺酸树脂(PFAR)及其前体全氟磺酰氟树脂(PFSR),以及由其为基材制备的全氟磺酸离子交换膜(PFSIEM)是重要的氟化工产品,在氯碱工业、燃料电池、化工生产和国防安全等领域有重要应用。介绍了PFSR,PFAR和PFSIEM的发展历程、产品种类、制备方式、加工方法、表征方法和产品应用,并对其研究热点及我国在该领域的发展进行了展望。 Perfluorosulfonic acid resin (PFAR) and its precursor,perfluorinated sulfonyl fluoride resin (PFSR),as well as perfluorosulfonate ion-exchanged membrane (PFSIEM) derived from them are important fluorinated chemical products.They play key roles in the fields of chlor-alkali industry,fuel cell,chemical production as well as national defense and state security.Herein,the development course,type of products,way for the preparation and method for the processing,the characterization methods as well as applications of PFSR,PFAR and PFSIEM were described.Finally,the focused points in the research work field as well as outlook for the development in China were presented. 参考文献 | 相关文章 | 计量指标

开发与应用

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磺酸盐型Gemini表面活性剂复配体系的黏度性质研究 Study on the viscosity characteristics of blend surfactant system containing sulfonate type Gemini surfactant 邹华,刘华荣,梅平 2016 (9):  502-506.  doi: 10.13218/j.cnki.csdc.2016.09.003 摘要 ( 286 )   PDF(763KB) ( 384 )   对以溴代十四烷、乙二胺和1,3-丙磺内酯为原料合成的磺酸盐型Gemini表面活性剂的表面活性进行了评价。主要研究了不同碳链长度的季铵盐、无机盐和有机盐的加入,剪切时间以及温度对上述表面活性剂体系黏度性质的影响。结果表明,磺酸盐型Gemini表面活性剂的临界胶束浓度比相应的单链表面活性剂低1~2个数量级;当向质量分数为1%的磺酸盐型Gemini表面活性剂中加入季铵盐时,复配体系的黏度先增加后减少,且季铵盐的碳链越长,增黏效果越明显,复配体系的黏度最大可达245.5 mPa·s,碳链的增长有助于蠕虫状胶束的形成;在磺酸盐型Gemini表面活性剂和十六烷基三甲基溴化铵(CTAB)的复配体系中,随着KCl,NaCl以及水杨酸钠质量分数的增加,复配体系的黏度先增加后减少,其中KCl的增黏效果最为显著,当KCl的质量分数为0.12%,复配体系的黏度达到最大,为430.2 mPa·s;在磺酸盐型Gemini表面活性剂/CTAB/KCl的复配体系中,随着剪切时间和温度的增加复配体系的黏度逐渐降低。 Evaluation of surface activity of a sulfonate type Gemini surfactant made of 1-bromotetradecane,ethylenediamine and 1,3-propane sultone was conducted.Effects of separate addition of quaternary ammonium salts (QASs) with different carbon chain length,inorganic salts,and organic salt,as well as shearing time period and temperature on the viscosity characteristics of the blend surfactant system containing the abovesaid sulfonate type Gemini surfactant were emphatically investigated.The results showed that the critical micelle concentration of above-mentioned surfactant is lower 1~2 order of magnitude than that of the corresponding single chain surfactant.When QASs is added into the sulfonate type Gemini surfactant aqueous solution of mass fraction of 1%,the viscosity of the blend surfactant system increases firstly;and the longer the carbon chain length of the QASs,the more obvious the viscosity increase effect;while up to a maximum value of 245.5 mPa·s,then it declines.Increase of the length of carbon chain helps the formation of wormlike micelles.The separate addition of KCl,NaCl and sodium salicylate all can increase the viscosity of the blend system composed of the sulfonate type Gemini surfactant and cetyltrimethylammonium bromide (CTAB) firstly and then decline.Among them,the most obvious one is KCl.When its mass fraction achieves 0.12%,the viscosity increases to a maximum value of 430.2 mPa·s.Following the increase of shearing time period and temperature,the viscosity of the blend system declines. 参考文献 | 相关文章 | 计量指标

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基于地沟油的双酯类阳离子表面活性剂及其降解行为 A diester type cationic surfactant based on waste oil from trench sewer and its degradation behavior 苗宗成,任建伟,冀静,赵阳,陈艳美 2016 (9):  507-510.  doi: 10.13218/j.cnki.csdc.2016.09.004 摘要 ( 291 )   PDF(777KB) ( 393 )   以地沟油为基本原料,经过水解、环氧氯丙烷开环酯化、与油酸脱水酯化、季铵化等化学过程,制备了一种新型的基于地沟油的双酯类阳离子表面活性剂;使用傅里叶变换红外光谱对产物的特征基团进行表征,并进一步使用表面张力仪和电导率仪测定产物的临界胶束浓度;最后采用好氧活性污泥法考察了所制备表面活性剂的降解行为。 A novel diester type cationic surfactant was prepared with waste oil collected from trench-sewer as raw material via chemical processes as hydrolysis,open-ring esterification with epichlorohydrin,esterification with oleic acid,and quaternization.FT-IR was used to characterize the chemical groups of the product.Moreover,the critical micelle concentration of the product was determined by surface tension method and electrical conductivity method.Finally,the degradation behavior of the cationic surfactant product was examined by aerobic sludge method. 参考文献 | 相关文章 | 计量指标

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不同农药助剂的初级生物降解性研究 Study on primary biodegradability of different pesticide adjuvants 孔祥吉,卜元卿,郭欣妍,单正军 2016 (9):  511-513.  doi: 10.13218/j.cnki.csdc.2016.09.005 摘要 ( 266 )   PDF(724KB) ( 483 )   以新型复配农药助剂——松脂基表面活性剂1号和2号以及传统农药助剂壬基酚聚氧乙烯醚、松香酸聚乙二醇酯和直链十二醇聚氧乙烯醚为目标物,通过实验考察了不同类型农药助剂的初级生物降解特性。8 d的生物降解实验结果表明,松脂基表面活性剂1号的初级生物降解度为79.1%,松脂基表面活性剂2号的初级生物降解度为82.4%,松香酸聚乙二醇酯的初级生物降解度为84.2%,壬基酚聚氧乙烯醚的初级生物降解度为91.1%,直链十二醇聚氧乙烯醚的初级生物降解度大于99%。新型复配农药助剂的组成结构更为复杂,其初级生物降解度要低于直链醇类、酚类的聚氧乙烯醚及单一结构酸类的聚乙二醇酯等农药助剂。 Primary biodegradability of the new blend pesticide adjuvants,rosin-based surfactant adjuvants No.1 and No.2,as well as that of the conventional pesticide adjuvants,including polyoxyethylene nonylphenol ether,rosin acid polyethylene glycol ester,and polyoxyethylene lauryl alcohol ether was investigated in laboratory tests of 8 d.The results indicated that primary biodegradability of rosin-based surfactant adjuvants No.1 is 79.1%,that of No.2 is 82.4%,that of rosin acid polyethylene glycol ester is 84.2%,that of polyoxyethylene nonylphenol ether is 91.1%,and that of polyoxyethylene lauryl alcohol ether is higher than 99%.It is obvious that the chemical structure of the new blend pesticide adjuvants is more complex and with lower primary biodegradability as comparing with that of the conventional pesticide adjuvants. 参考文献 | 相关文章 | 计量指标

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神经酰胺ⅢB纳米脂质体的制备及功效评价 Preparation and efficacy evaluation of ceramide ⅢB nanoliposome 李霞,田仁德,许琦,郭凤凤,刘卫 2016 (9):  514-518.  doi: 10.13218/j.cnki.csdc.2016.09.006 摘要 ( 478 )   PDF(2829KB) ( 418 )   采用高压匀质技术制备了神经酰胺ⅢB纳米脂质体,平均粒径为71.7 nm,PDI(多分散性系数)为0.214,Zeta电位为-23.3 mV,载药量和包封率分别为2.3%和95.9%。采用Franz扩散池法考察了其体外透皮性能,结果显示,其24 h体外皮肤累积透过量为709.23 μg/cm2,皮肤滞留量为75.07 μg/cm2。相同神经酰胺ⅢB质量分数的纳米脂质体霜剂与普通霜剂相比,前者24 h皮肤滞留量提高了近6倍。比较了连续给药40 d前后小鼠皮肤的水合能力,结果显示,神经酰胺ⅢB纳米脂质体组小鼠皮肤水合能力较对照组有明显提高,小鼠皮肤中总神经酰胺质量浓度高于对照组。 Ceramide ⅢB nanoliposome was prepared by high pressure homogenization technique.Properties of the product were measured as particle size,71.7 nm;PDI,0.214;Zeta potential,-23.3 mV;rate of drug loading,2.3%;rate of encapsulation,95.9%.The in vitro skin permeation and retention tests were performed with Franz diffusion cell method.Results showed that the cumulative permeation and skin retention in 24 h was 709.23 and 75.07 μg/cm2,respectively.The skin retention of ceramide ⅢB nanoliposome cream product in 24 h was 6 times higher than that of conventional ceramide ⅢB cream product with the same mass fraction.The experiment was continued for 40 d on mouse skin and the results demonstrated that ceramide ⅢB nanoliposome exhibits a significant epidermal hydration capacity and total ceramides mass concentration as comparing with that of the control test group. 参考文献 | 相关文章 | 计量指标

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桑黄提取物体外美容功效研究 Study on beautifying effects of Phellinus linteus extract in vitro 沈雪梅,王荣庆,王雪梅,赵玮,肖伟莉 2016 (9):  519-523.  doi: 10.13218/j.cnki.csdc.2016.09.007 摘要 ( 364 )   PDF(944KB) ( 408 )   通过紫外吸收效果评价了桑黄提取物的防晒性能;通过酪氨酸酶、透明质酸酶抑制实验和DPPH自由基清除法评价了桑黄提取物的美白、抗敏和抗氧化功效;通过建立体外非酶糖化反应体系,考察了桑黄提取物对糖化反应的抑制作用。结果表明:桑黄醇提物在UVA波段具有很强的吸收能力,且具有很好的美白、抗敏及抗氧化功效,还能够有效抑制Amadori(早期糖化产物)和AGEs(高级糖化终末产物)的形成;桑黄水提物具有一定的抗敏和抗氧化功效,能够有效抑制AGEs的形成。 The sunscreening performance of Phellinus linteus extracts (including alcohol extract and aqueous extract) was evaluated based on their ultraviolet absorption efficacy.Their whitening and anti-allergic effects were evaluated by tyrosinase and hyaluronidase inhibition test respectively.Their anti-oxidation effect was measured with DPPH free radical scavenging method.Their inhibitory effect on glycation was studied by establishing a non-enzymatic glycation reaction system in vitro.Results showed that Phellinus linteus alcohol extract displays a strong capacity for absorbing ultraviolet energy within UVA band,as well as excellent whitening,anti-allergic and anti-oxidation effect.It can also effectively inhibit the formation of Amadori (early stage product of glycation) and AGEs (end products of glycation).Phellinus linteus aqueous extract displays a certain anti-allergic and anti-oxidation effect,and can effectively inhibit the formation of AGEs. 参考文献 | 相关文章 | 计量指标

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运载辅酶Q10的纳米结构脂质载体在化妆品中的应用 Application of co-enzyme Q10-loaded nanostructured lipid carriers in cosmetics 梁蓉,吴丽娜,杨成,钱鑫,曹光群 2016 (9):  524-529.  doi: 10.13218/j.cnki.csdc.2016.09.008 摘要 ( 328 )   PDF(2240KB) ( 315 )   考察了经水溶性季铵盐壳聚糖(QCS)修饰后的辅酶Q10 (CoQ10)纳米结构脂质载体(QCS-CoQ10-NLC)在护肤乳霜中的应用品质。结果显示:纳米结构脂质载体(NLC)的添加并未对护肤乳霜的耐热、耐寒及离心稳定性产生影响,护肤乳霜稳定性良好;与添加了等量游离CoQ10和未包埋CoQ10的空白QCS-NLC护肤乳霜相比,添加QCS-CoQ10-NLC的护肤乳霜能有效降低乳霜在冷热交替及光照储藏过程中CoQ10的降解,显著提高其保留率。此外,护肤乳霜的保湿性测试和感官评价测试结果显示,QCS-CoQ10-NLC的添加能有效提高其保湿性和感官性能。 Application characteristics of co-enzyme Q10 (CoQ10)-loaded nanostructured lipid carriers (NLC) modified with water soluble quaternized chitosan (QCS-CoQ10-NLC) in skin care emulsion cosmetics were examined.Results showed that the addition of NLC does not affect the stability of skin care emulsion cosmetics through heat resistance test,low temperature resistance test and centrifugation test.As comparing with the skin care emulsion cosmetics containing the same amount of free CoQ10 and blank QCS-NLC without CoQ10 loading,the degradation of CoQ10 in the skin care emulsion cosmetics containing QCS-CoQ10-NLC is less under the alternative heat-low temperature test and illumination storage test,with a significant increasing of retention rate.In addition,the moisture test and sensory evaluation showed that the addition of QCS-CoQ10-NLC could enhance the moisture retention and sensory properties of the skin care emulsion cosmetics. 参考文献 | 相关文章 | 计量指标

专论与综述

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日用化学品用合成麝香 Synthetic musk in daily chemicals 周静 2016 (9):  530-538.  doi: 10.13218/j.cnki.csdc.2016.09.009 摘要 ( 412 )   PDF(873KB) ( 1017 )   简要介绍了合成麝香的分类及其代表物质,综述了目前合成麝香的毒性研究成果,比较了我国和欧盟对于合成麝香在化妆品中添加量的法规限定,阐述了日化产品中合成麝香的主要前处理和仪器检测方法,并对未来合成麝香的研究进行了展望。 The classification and the typical compounds of synthetic musk were briefed.The research work results with respect to toxicity of synthetic musk were reviewed.Regulations for the limitations of application of synthetic musk in cosmetics executed in China and the European Union were compared.The main pretreatment and instrument detection methods for synthetic musk applied in cosmetics were described and the development trends were prospected. 参考文献 | 相关文章 | 计量指标

分析与检测

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氢化物-原子荧光光谱法测定化妆品粉质原料中4种有害重金属 Detection of four kinds of harmful heavy metal in powder form raw materials used for cosmetics by hydride generation atomic fluorescence spectrometry 杨慧敏,封棣,孙丽丽,孟伟光,魏耀辉 2016 (9):  539-543.  doi: 10.13218/j.cnki.csdc.2016.09.010 摘要 ( 234 )   PDF(796KB) ( 352 )   建立了一种测定化妆品粉质原料中Pb,Hg,As和Cd 4种重金属元素的湿式消解-氢化物发生原子荧光光谱法。通过比较湿式消解法和干灰化法的加标回收率,结果显示,湿式消解法更适合4种重金属元素的前处理。在较优的实验条件下,湿式消解-氢化物发生原子荧光光谱法测定Pb,Hg,As和Cd的线性范围分别为0～16.0,0～1.6,0～16.0和0～1.6 μg/L,相关系数(R2)为0.993 5～0.999 7,方法检出限为0.036～0.768 μg/L,样品加标回收率为81.0%～93.0%。该方法灵敏度高,精密度和准确度好,满足分析要求。同时利用该方法实际检测了10种化妆品粉质原料。 A detection method of lead,mercury,arsenic and cadmium in powder form raw materials used for cosmetics was established by hydride generation atomic fluorescence spectrometry with wet digestion method as the sample pretreatment.Comparison of spiked recoveries of wet digestion method and dry calcination method showed that the wet digestion method is more suitable for sample preparation.Under the optimized conditions,the linearity range of lead,mercury,arsenic and cadmium are 0-16.0,0-1.6,0-16.0 and 0-1.6 μg/L respectively.The correlation coefficients (R2) are from 0.993 5 to 0.999 7;the detection limits are from 0.036 to 0.768 μg/L;the spiked recoveries are from 81.0% to 93.0%.The method is sensitive,accurate and precise for the detection of heavy metals and has been successfully applied to detect lead,mercury,arsenic and cadmium in 10 kinds of powder form raw material used for preparation of cosmetics. 参考文献 | 相关文章 | 计量指标

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双波长HPLC法同时测定植物防晒复配物中7种防晒成分的含量 Simultaneous determination of seven kinds of sunscreen component in blend of plant extract by RP-HPLC 岳爱国,刘纲勇,王如意,刘经亮 2016 (9):  544-548.  doi: 10.13218/j.cnki.csdc.2016.09.011 摘要 ( 294 )   PDF(907KB) ( 394 )   建立了双波长高效液相色谱法(RP-HPLC)同时测定自制植物防晒复配物中绿原酸、芦丁、黄芩苷、丹皮酚、黄芩素、大黄素和大黄酚7种防晒成分的含量。样品用纯甲醇溶解,采用WondaSil C18 WR色谱柱(250 mm×4.6 mm,5 μm)分离,以甲醇和0.1%磷酸溶液为流动相进行梯度洗脱,流速1.0 mL/min,检测波长270和327 nm,柱温40 ℃。结果表明,绿原酸、芦丁、黄芩苷、丹皮酚、黄芩素、大黄素和大黄酚的线性范围分别为4.24~42.4,6.76~67.6,4.16~41.6,4.90~49.0,4.34~43.4,4.28~42.8和5.72~57.2 ng,线性相关系数均大于0.999。7种防晒成分的平均回收率为 92.4%~107.8%,RSD为3.81%~7.38%。该方法操作简便、准确、重复性好,可用于自制植物防晒复配物的质量控制。 A RP-HPLC method was established for simultaneous determining chlorogenic acid,lutin,baicalin,paeonol,baicalein,emodin and chrysophanol in blend of plant extract.The sample was extracted by high purity methanol.The separation was performed on a WondaSil C18 WR column (250 mm×4.6 mm,5 μm);with methanol and 0.1% H3PO4 solution as mobile phase.The flow rate was 1.0 mL/min,the detection wavelength was 270 and 327 nm,and the column temperature was 40 ℃.Results showed that,the linearity ranges within 4.24-42.4 ng for chlorogenic acid,6.76-67.6 ng for lutin,4.16-41.6 ng for baicalin,4.90-49.0 ng for paeonol,4.34-43.4 ng for baicalein,4.28-42.8 ng for emodin,and 5.72-57.2 ng for chrysophanol and all correlation coefficients are higher than 0.999.The average spiked recovery rates are from 92.4% to 107.8%,and the relative standard deviations (RSD) are from 3.81% to 7.38%.The method is simple,accurate and suitable for the quality control for the preparation of such blend plant extracts. 参考文献 | 相关文章 | 计量指标