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    2017年, 第47卷, 第7期 刊出日期:2017-07-22 上一期    下一期
    基础研究
    PVP-SDS缔合行为与pH及比浓黏度的关系
    Relationship between association behavior of PVP-SDS and the change of pH or reduced specific viscosity
    吴业帆, 奚丽莎, 方云, 林梦楚, 李秀秀, 翟然
    2017 (7):  361-364.  doi: 10.13218/j.cnki.csdc.2017.07.001
    摘要 ( 402 )   PDF(764KB) ( 352 )  
    非离子聚合物-阴离子表面活性剂溶液的pH和黏度随体系内分子聚集形态的不同而发生改变,据此建立pH法和比浓黏度法研究了聚乙烯吡咯烷酮(PVP)与不同浓度十二烷基硫酸钠(SDS)的缔合行为,结果表明2种方法均可表征PVP-SDS的双临界浓度。比浓黏度曲线上的极小值和极大值使比浓黏度法具有很高的灵敏性和准确性,而pH法表明氢离子对PVP-SDS缔合行为有重要作用。 Methods by means of pH and reduced specific viscosity measurement were established to study polyvinylpyrrolidone (PVP)-sodium dodecylsulfate (SDS) association under various concentrations of SDS since pH and viscosity of the system are sensitive to aggregation behaviors.It is the fact that double critical concentrations of SDS in the PVP-SDS association can be characterized by both methods.The reduced specific viscosity method is more sensitive and accurate than the pH method for both the minimum and the maximum values appeared on reduced specific viscosity plots corresponding to double critical concentrations of SDS,whereas the advantage of the pH method is to support the important effect of hydrogen ion on establishment of the PVP-SDS association.
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    科技讲座
    离子液体表面活性剂的合成与应用(Ⅶ)——在化学反应中的应用
    Synthesis and application of ionic liquid surfactants (Ⅶ) Applications of ionic liquid surfactants in chemical reactions
    徐清杰, 杨许召, 王萍, 邹文苑, 王军
    2017 (7):  365-368.  doi: 10.13218/j.cnki.csdc.2017.07.002
    摘要 ( 279 )   PDF(926KB) ( 364 )  
    离子液体表面活性剂同时具有有机溶剂的属性和优良的表面活性,有利于促进化学反应的进行。离子液体表面活性剂能提高酶的活力,促进酶催化反应。Lewis和Brönsted酸型离子液体表面活性剂能高效催化Ullmann耦合反应和酯化反应。表面活性剂/多金属氧酸盐和表面活性剂/过氧酸分别成功催化了油品的氧化脱硫反应和烯烃的环氧化反应。离子液体表面活性剂通过降低溶液的表面张力和环状阳离子架构水合物笼的模板作用促进了CO2水合物的快速生成。 Because of the dual properties of organic solvent and excellent surface activity,ionic liquid surfactants are used to accelerate chemical reactions.Enzymatic reaction is enhanced with improved enzyme activity greatly by ionic liquid surfactants.Lewis acidic and Brönsted acidic ionic liquid surfactants are used to catalyze Ullmann-type coupling and esterification reactions.Poly-metal salts of oxy-acid or per-oxy acid,in combination with surfactant has been used separately to catalyze oxidation desulfurization of petroleum fractions and epoxidation of oleffins.CO2 hydrate is quickly formed by decreasing of the surface tension with ionic liquid surfactants and template action of cyclic cationics.
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    开发与应用
    胺基CO2开关型表面活性剂的合成与性能研究
    Synthesis and performance of CO2 switchable amine surfactants
    张鹏, 梅平, 赖璐
    2017 (7):  369-373.  doi: 10.13218/j.cnki.csdc.2017.07.003
    摘要 ( 263 )   PDF(1122KB) ( 383 )  
    以溴代十四烷和二乙烯三胺为原料,合成了表面活性剂十四烷基二乙烯三胺(C14DETA)。采用红外光谱和核磁共振氢谱对C14DETA进行了结构表征。通过研究其电导率可逆、pH可逆和与SDS协同作用的开启,证明了C14DETA具有良好的CO2开关性能。测定了十四烷基二乙烯三胺碳酸氢盐(C14DETA-CO2)和SDS/C14DETA-CO2复配体系的临界胶束浓度,分别为1.0×10-2和1.0×10-4 mol/L。通过测定C14DETA-CO2对正癸烷/水体系的乳化性能,证明了C14DETA-CO2具有良好的乳化性能,所制得乳状液为W/O型,其较佳乳化条件为:C14DETA-CO2的质量分数4%,油水体积比1∶1或1∶2。 Surfactant tetradecyldiethylenetriamine (C14DETA) was synthesized with 1-bromotetradecane and diethylenetriamine as starting materials.Its structure was characterized by FT-IR and 1H NMR spectrum.Measurement of reversibility of conductivity,reversibility of pH values,and the opening action of synergistic effect with SDS demonstrate the good CO2 switchability of C14DETA.The critical micelle concentrations (cmc) of tetradecyldiethylenetriamine bicarbonate (C14DETA-CO2) and the mixed system of SDS/C14DETA-CO2 are 1.0×10-2 and 1.0×10-4 mol/L respectively.Results of emulsifying performance of C14DETA-CO2 for n-decane/water system prove the good emulsifying power of C14DETA-CO2.The emulsion is water-in-oil type,and its better emulsifying conditions are:mass fraction of C14DETA-CO2,4%;and the volume ratio of oil/water,1∶1 or 1∶2.
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    疏水缔合型阳离子聚丙烯酰胺的合成及絮凝性能
    Synthesis and flocculation performance of hydrophobically associating cationic polyacrylamide
    郭睿, 王映月, 郭煜
    2017 (7):  374-378.  doi: 10.13218/j.cnki.csdc.2017.07.004
    摘要 ( 350 )   PDF(1024KB) ( 443 )  
    以甲基丙烯酸三氟乙酯(TFEMA)为疏水单体、丙烯酰胺(AM)为主单体、甲基丙烯酰氧乙基三甲基氯化铵(DMC)为阳离子单体,以过硫酸铵和亚硫酸氢钠为复合引发剂,采用自由基胶束聚合法合成了共聚物P(AM-DMC-TFEMA)。分别考察了反应温度、引发剂用量、单体总质量分数及反应时间对P(AM-DMC-TFEMA)的产率及阳离子度的影响。确定较佳工艺条件为:反应温度65 ℃,引发剂用量占单体总质量的2%,单体总质量分数26%,反应时间3 h。采用红外光谱(FT-IR)、核磁共振氢谱(1H NMR)和环境扫描电镜(ESEM)对其结构进行了表征。同时考察了P(AM-DMC-TFEMA)对硅藻土悬浮液的絮凝效果,结果表明,其对硅藻土具有良好的絮凝效果,絮凝时间仅为20 s,合成的共聚物上清液透过率为97.31%。 With trifluoroethyl methacrylate (TFEMA) as the hydrophobic monomer,acrylamide (AM) as main monomer,methacryloxyethyltrimethylammonium chloride (DMC) as cationic monomer,ammonium persulfate and sodium bisulfite as composite initiator,the product copolymer P(AM-DMC-TFEMA) was synthesized using free radical micellar copolymerization method.Effects of reaction temperature,initiator dosage,mass fraction of total monomers and reaction time on the yield and level of cationization of P(AM-DMC-TFEMA) were examined.Better process conditions are suggested as following:reaction temperature,65 ℃;dosage of initiator,2% of total mass of the monomers;mass fraction of total monomers,26%;reaction time,3 h.The structure of the product was characterized by infrared spectroscopy (FT-IR),1H nuclear magnetic resonance (1H NMR) and environmental scanning electron microscopy (ESEM).Meanwhile,the flocculation effect of the product P(AM-DMC-TFEMA) on diatomaceous earth suspension was also examined.Results show that P(AM-DMC-TFEMA) displays good flocculation effect on diatomaceous earth,the flocculation time is only 20 s,and the ratio of the clear copolymer product liquid achieves 97.31%.
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    利用双头季铵盐合成特殊形貌的EU-1分子筛及其催化性能
    Synthesis of EU-1 zeolites with special morphology using double-headed quaternary ammonium salt and their catalytic performance
    高李霞, 李晓峰, 高萌, 刘晓臻, 李国栋, 窦涛
    2017 (7):  379-383.  doi: 10.13218/j.cnki.csdc.2017.07.005
    摘要 ( 283 )   PDF(2046KB) ( 330 )  
    以双头季铵盐C18-6-6Br2为辅助模板剂,分别通过水热法和蒸汽相法合成了具有特殊形貌的EU-1分子筛。利用XRD、SEM、NH3-TPD和N2吸附-脱附等手段对样品进行表征,使用二甲苯异构化作为探针反应进行催化性能评价。结果表明:双头季铵盐C18-6-6Br2的加入可明显改变EU-1分子筛的形貌,尤其在蒸汽相条件下作用效果更为显著,合成的EU-1分子筛形貌呈蜂巢形,同时其强酸量和弱酸量下降,总比表面积和总孔体积分别增加了83.65%和126.72%,二甲苯异构化反应中对二甲苯(PX)收率、选择性(Y(C8))和催化活性([PX]/ΣX)均显著提高,分别增加了8.94%,6.44%和6.01%。 Using double-headed quaternary ammonium salt C18-6-6Br2 as the assistant template,the EU-1 zeolites with special morphology were synthesized with hydrothermal method and vapor phase method.The product samples were characterized by XRD,SEM,NH3-TPD and N2 adsorption-desorption.Besides,xylene isomerization was used as the probe reaction to evaluate their catalytic performance.Results show that the addition of the double-headed quaternary ammonium salt C18-6-6Br2 can effectively change the morphology of the product,especially in the case of vapor phase method.The morphology of EU-1 zeolite synthesized by adding C18-6-6Br2 in the steam phase shows honeycomb,and both its strong acid content and weak acid content decrease.The total specific surface area and the total pore volume increases by 83.65% and 126.72% respectively.The yield of xylene (PX),the selectivity (Y(C8)) and the catalytic activity ([PX]/ΣX) significantly increases by 8.94%,6.44% and 6.01% respectively in the xylene isomerization reaction.
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    聚甘油酯化改性PMVE/MAH的合成及吸水性能研究
    Synthesis and water-retaining performance of poly(methyl vinyl ether-co-maleic anhydride)/polyglycerol
    周铮鸣, 陈洪龄
    2017 (7):  384-388.  doi: 10.13218/j.cnki.csdc.2017.07.006
    摘要 ( 302 )   PDF(769KB) ( 254 )  
    以甲基乙烯基醚/马来酸酐共聚物(PMVE/MAH)与十聚甘油为原料,采用溶剂接枝法,制得聚甘油酯化改性PMVE/MAH。采用红外光谱和热分析仪对酯化产物进行了结构表征。研究了反应酯化率对产物性能的影响,考察了产物的热稳定性、保水性能、耐电解质性和重复吸水性能。结果表明,酯化率12.5%的共聚物吸水性最强,pH=7时吸水倍率为353 g/g,最适宜酸碱性条件为pH=8,此时酯化改性共聚物吸水倍率可达719 g/g,耐盐性良好,50 ℃环境温度下16 h 仍有67.2%的保水率。 Poly(methyl vinyl ether-co-maleic anhydride)/polyglycerol water-retaining agent was prepared by esterification of poly(methyl vinyl ether-co-maleic anhydride) (simplified expressed as PMVE/MAH) and decaglycerol with solution-grafting method.Structure of the esterified product was characterized by FT-IR and thermo-gravimetric analysis.The effect of esterification rate on performance of the product were examined.In addition,thermal stability,water retention capacity,electrolyte resistance and reuse ability of the product were studied.Results show that the copolymer with the esterification rate of 12.5% displays the strongest water absorption,which achieves 353 g/g at pH=7 with good salt resistance;and the water absorption of the copolymer reaches 719 g/g at pH=8.Under the environment temperature 50 ℃ for 16 h,the water retention rate still achieves 67.2% of the original water retention rate.
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    鲑鱼皮胶原蛋白肽的保湿性研究
    Study on moisturizing efficacy of collagen peptides from salmon skin
    孔惠, 邢晓平, 孙安琪, 曹玉华, 曹光群
    2017 (7):  389-393.  doi: 10.13218/j.cnki.csdc.2017.07.007
    摘要 ( 463 )   PDF(764KB) ( 329 )  
    以鲑鱼皮为原料,采用酸浸-水提法得到鲑鱼皮明胶,并通过酶解制备了鲑鱼皮胶原蛋白肽,其中超过91.5%的鲑鱼皮胶原蛋白肽分子量小于1 000 Da。通过葡聚糖凝胶G-15层析柱分离出5种组分,按其分子量的大小依次为:S1>S2>S3>S4>S5。体外试验结果表明,相对湿度81%的环境下,吸湿性顺序为:S5>S4>甘油>鲑鱼皮胶原蛋白肽>S3>S2>S1≈透明质酸>鲑鱼皮明胶;保湿性顺序为:S5≈S4>S3>S2>甘油>鲑鱼皮胶原蛋白肽>S1>透明质酸>鲑鱼皮明胶。相对湿度43%的环境下,吸湿性顺序为:S5>甘油>S4>鲑鱼皮胶原蛋白肽≈S3>透明质酸>S2>S1>鲑鱼皮明胶;保湿性顺序为:S5>S4>甘油>S3≈鲑鱼皮胶原蛋白肽>透明质酸≈S2>S1>鲑鱼皮明胶。皮肤测试结果表明,涂抹含鲑鱼皮胶原蛋白肽的护肤品能够显著提高皮肤水分含量和降低经表皮失水率(TEWL),小分子鲑鱼皮胶原蛋白肽的保湿效果优于鲑鱼皮明胶。 Gelatin was extracted from salmon skin (hereinafter refers to as the gelatin) by acid leaching and water extraction.Then the gelatin were hydrolyzed enzymatically to prepare collagen peptides.More than 91.5% of the collagen peptides has a molecular weight of less than 1 000 Da.Five fractions from collagen peptides named S1,S2,S3,S4,S5 in decreasing order of molecular weight were separated by sephadex G-15.The study in vitro shows that when RH was 81%,the moisture absorption is a decreasing sequence as S5>S4>glycerol>collagen peptides>S3>S2>S1≈hyaluronic acid>the gelatin.The moisturizing effect shows a tendency of S5≈S4>S3>S2>glycerol>collagen peptides>S1>hyaluronic acid>the gelatin.When RH was 43%,the moisture absorption is a decreasing sequence as S5>glycerol>S4>collagen peptides≈S3>hyaluronic acid>S2>S1>the gelatin.The moisturizing effect is S5>S4>glycerol>S3≈collagen peptides>hyaluronic acid≈S2>S1>the gelatin.The skin test results show that collagen peptides from salmon skin significantly increase skin hydration and effectively decrease transepidermal water loss (TEWL),which is superior to that of the gelatin from salmon skin.
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    基于多重乳化体技术制备中草药防晒霜
    Preparation of sun-screening cosmetic cream containing Chinese traditional herb medicine based on multiple emulsion technology
    孟潇, 许锐林, 陈庆生, 龚盛昭
    2017 (7):  394-397.  doi: 10.13218/j.cnki.csdc.2017.07.008
    摘要 ( 324 )   PDF(735KB) ( 286 )  
    采用乙醇提取罗勒等7种中草药,将制备的各单一中草药提取液等质量混合,制得中草药提取液组合物。通过紫外分光光度法对其紫外线吸收率进行测定,结果表明其具有较佳紫外线吸收效果。分别采用4种脱色剂活性炭、高锰酸钾、过氧化氢和草酸对其进行脱色研究,结果表明,经草酸脱色后的中草药提取液组合物颜色较浅,且仍保持较好的紫外线吸收效果。基于多重乳化体技术,将制备的中草药提取液组合物添加于W/O/W型多重乳化体的最内相中,制备得到中草药防晒霜,并与单重乳化体中草药防晒霜进行比较。测试评价结果表明,多重乳化体中草药防晒霜具有较好的温和性和稳定性,当中草药提取液组合物添加量为15.0%时,SPF和PFA值分别为20.3和5.3。 Ethanol extraction method was used to extract seven kinds of Chinese traditional herb medicine (CTHM),including Ocimum basilicum et al.The extracts of CTHM were blended in accordance with equal mass to prepare blend extracts.UV spectrophotometry was used to determine the UV absorbance of the blend extracts.Results show that it has better UV absorption effect.Four decolorizing agents,activated carbon,KMnO4,H2O2,and oxalic acid were tested to determine the best decolorizing agent.Results show that oxalic acid displays good decolorizing effect and retains the UV absorbance significantly.Then the blend extracts wasformulated in the cosmetic cream based upon multiple emulsion technology with the blend extracts introduced into the internal phase of the W/O/W emulsion.Evaluation results show that,as comparing with that of the single emulsion,the multiple emulsion is more mild and stable,and when the dosage of the blend extracts achieves 15.0%,the value of SPF and PFA can achieve 20.3 and 5.3 respectively.
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    羊栖菜岩藻多糖的提取工艺优化及保湿性能
    Optimization of process technological conditions for obtaining fucoidan from Sargassum fusiforme and detection of its moisturizing performance
    刘冰月, 刘学, 邬凤娟, 曹光群, 张晨, 杨杰
    2017 (7):  398-402.  doi: 10.13218/j.cnki.csdc.2017.07.009
    摘要 ( 373 )   PDF(789KB) ( 310 )  
    以脱脂羊栖菜为原料,采用纤维素酶酶解-超声波辅助法提取羊栖菜岩藻多糖(FSF)。通过正交试验对提取条件进行优化,考察提取液pH、纤维素酶用量、提取温度、酶解时间和超声时间对FSF提取率的影响,结果表明较佳提取条件为:pH=4.5,纤维素酶用量为脱脂羊栖菜样品质量的1.0%,提取温度40 ℃,酶解时间2 h,超声时间15 min,料液比 1∶10 (g∶mL),在此条件下,FSF的提取率为8.50%,相对标准偏差为2.74%。在相对湿度为43%和81%的条件下,羊栖菜岩藻多糖粗提取物(CEFSF)的短效吸湿性(8 h)优于甘油、丁二醇及海藻酸钠;质量分数为1%的CEFSF溶液的保湿性能优于质量分数为1%的丁二醇或海藻酸钠溶液,与质量分数为5%的甘油溶液相当。皮肤水分含量测定和经表皮水分散失速率测定结果表明:质量分数为5%的CEFSF溶液具有良好的保湿效果。 Process technological conditions for obtaining fucoidan from Sargassum fusiforme (FSF) via ultrasonic assisted enzymatic hydrolysis with cellulase was optimized by orthogonal experiments.Factors that affect the yield of FSF,including solvent pH value,enzyme dosage,reaction temperature,cellulase hydrolysis time,and ultrasonic time were investigated.The better extraction conditions were as following:pH,4.5;enzyme dosage,1% of the mass of the raw material;reaction temperature,40 ℃;cellulase hydrolysis time,2 h;ultrasonic time,15 min;and material-liquid ratio,1∶10 (g∶mL).Under such conditions,the yield of FSF achieves 8.50%,and RSD=2.74%.The hygroscopicity (8 h) of crude extract of fucoidan from Sargassum fusiforme (CEFSF) is better than that of glycerin,butanediol,and sodium alginate.The moisture retention capacity of 1% CEFSF aqueous solution (mass fraction) is better than 1% butanediol (mass fraction) and 1% sodium alginate (mass fraction),which is equivalent to that of 5% glycerin (mass fraction),under relative humidity of 43% and 81%.The results of skin moisture content and transepidermal water loss rate show that:5% CEFSF aqueous solution (mass fraction) shows a good moisturizing effect.
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    椰油酰基甘氨酸钾部分酸化对洁面膏性能的影响
    Performance of facial cleanser impacted by partial acidification of potassium cocoyl glycinate
    汤小芹, 陈明华, 李芳芳, 任天辉
    2017 (7):  403-407.  doi: 10.13218/j.cnki.csdc.2017.07.010
    摘要 ( 829 )   PDF(1935KB) ( 567 )  
    以柠檬酸为酸化剂,研究了洁面膏体系中椰油酰基甘氨酸钾的部分酸化对其结膏温度、料体黏度、膏体外观、微观状态、稳定性和泡沫性能的影响。结果表明,当用于调节酸化程度的柠檬酸的质量分数为1.4%~2.8%时,所得椰油酰基甘氨酸钾洁面膏的pH=6.68~7.02,产品的黏度约为100 Pa·s,结膏温度满足实际生产及应用要求,稳定性较好,膏体柔软、珠光细腻,泡沫丰富。 Citric acid was used as acidifier to examine the influence of partial acidification of potassium cocoyl glycinate on crystallizing temperature,viscosity,appearance,microstructure,stability and foam performance of the facial cleanser system.It was found that partially acidulated potassium cocoyl glycinate in which the addition of citric acid is between 1.4%-2.8% displays the optimized performance in facial cleanser (pH=6.68-7.02),which indicates proper crystallizing temperature,viscosity at about 100 Pa·s,good stability,soft paste feeling,bright pearly luster appearance,fine foam,and satisfies the requirements for its practical application in the cleansing system.
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    抗氧化菌的筛选及混菌发酵红景天条件优化
    Screening of antioxidant bacteria and optimization of conditions for fermentation of Rhodiola rosea with mixed bacteria
    戴玥, 余晓斌
    2017 (7):  408-413.  doi: 10.13218/j.cnki.csdc.2017.07.011
    摘要 ( 273 )   PDF(1543KB) ( 294 )  
    通过测定12株酵母菌的谷胱甘肽(GSH)含量、超氧化物歧化酶(SOD)活力和羟基自由基清除能力以及8株乳酸菌的总还原力和超氧阴离子自由基清除能力,分别筛选出抗氧化性强的产朊假丝酵母(酵母菌Y1)和干酪乳杆菌(乳酸菌L8)。比较了14种中药经混菌(酵母菌Y1和乳酸菌L8)发酵前后酪氨酸酶抑制率和总还原力的变化,得出红景天为最佳发酵中药。以红景天为原料,采用纤维素酶-果胶酶酶解后添加其他营养成分,以酪氨酸酶抑制率为指标,采用响应面法优化混菌发酵红景天的条件:葡萄糖质量分数12.35%、液料比18.67∶1 (mL∶g)、发酵时间5.25 d,在此条件下红景天发酵液酪氨酸酶抑制率为73.21%,比未发酵的提高了67.72%。 By determining the content of glutathione (GSH),SOD enzyme activity,and hydroxyl free radical scavenging ability of 12 yeast strains and total reducing capacity,and superoxide anion free radical scavenging ability of 8 lactic acid bacteria,Y1 (Candida utilis) and L8 (Lactobacillus casei) with high antioxidant activity were screened.The changes of tyrosinase inhibition rate and total reducing capacity of 14 kinds of Chinese traditional herb medicine with mixed bacteria (Y1 and L8) were compared before and after fermentation.Based upon test results,it is suggested that Rhodiola rosea (after fermentation) is the best Chinese traditional herb medicine to be used.Rhodiola rosea as the starting material is to be hydrolyzed by cellulase-pectinase complex enzyme;with tyrosinase inhibition rate as the index;the conditions for fermentation of Rhodiola rosea with mixed bacteria were optimized by using response surface methodology.Results indicate that the conditions of Rhodiola rosea fermented by mixed bacteria can be recommended as follows:glucose mass fraction,12.35%;liquid-solid ratio,18.67∶1 (mL∶g);fermentation time,5.25 d.Under such conditions,the tyrosinase inhibition rate achieves 73.21%,which is 67.72% higher than that before the fermentation.
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    专论与综述
    物理防晒剂在液相介质中的分散及稳定性
    Dispersion and stability of physical sun-screening agents in liquid medium
    邬凤娟, 张晨, 甘亮, 倪鑫炯, 李云兴, 曹光群
    2017 (7):  414-417.  doi: 10.13218/j.cnki.csdc.2017.07.012
    摘要 ( 436 )   PDF(691KB) ( 296 )  
    概述了物理防晒剂在液相介质中的分散过程和分散方法;介绍了超细颗粒在液相介质中的多种稳定机理,并对物理防晒剂粉浆的稳定机理进行探讨;最后列举了现有的物理防晒剂粉浆的稳定性评价方法。 The dispersion process and methods of physical sun-screening agents in liquid medium were briefed.Several stabilizing mechanisms for ultrafine particles in liquid medium were introduced,and the stabilizing mechanism for physical sun-screening slurry was discussed.At last,the currently existing evaluation methods of physical sun-screening slurry stability were illustrated.
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    分析与检测
    高效液相色谱法同时测定化妆品中5种防腐剂
    Simultaneous determination of five kinds of preservative in cosmetics by high performance liquid chromatography
    张卓娜, 林少彬, 杨艳伟
    2017 (7):  418-420.  doi: 10.13218/j.cnki.csdc.2017.07.013
    摘要 ( 245 )   PDF(740KB) ( 273 )  
    建立了同时测定化妆品中5种防腐剂的高效液相色谱分析方法。采用C18色谱柱(250 mm×4.6 mm,5 μm)分离,以甲醇-水为流动相,流速为1.0 mL/min,检测波长为230 nm,柱温25 ℃。结果表明,5种防腐剂的线性范围为0~200 mg/L,方法的线性关系良好,5种防腐剂氯苯甘醚、邻苯基苯酚、氯二甲酚、苄氯酚和三氯生的检出限分别为0.10,0.10,0.15,0.25和0.30 mg/L。样品的平均加标回收率为97.6%~115%,相对标准偏差为0.30%~1.65% (n=6)。 A high performance liquid chromatography method was established for determination of five kinds of preservative in cosmetics.A C18 column (250 mm×4.6 mm,5 μm) was used as stationary phase,and methanol aqueous solution was used as mobile phase with a flow rate of 1.0 mL/min.The detection wavelength was set at 230 nm and the column temperature was 25 ℃.The linearity range of the five kinds of preservative is 0-200 mg/L,and the method shows a good linear relationship.The detection limits for chlorphenesin,biphenyl-2-ol,chloroxylenol,chlorophene and triclosan achieve 0.10,0.10,0.15,0.25 and 0.30 mg/L respectively.The spiked recovery rate varies from 97.6% to 115%.The relative standard deviation achieves 0.30%-1.65% (n=6).
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