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Table of Content

    22 November 2014, Volume 44 Issue 11 Previous Issue    Next Issue
    Basic research
    Preparation and properties of poly[2-(N,N-dimethyl amino) ethyl methacrylate] with dodecyl group
    ZHOU Jian-hua, WANG Hai-long, HE Ren-yan
    2014, 44 (11):  601-604.  doi: 10.13218/j.cnki.csdc.2014.11.134
    Abstract ( 228 )   PDF (979KB) ( 374 )  
    Poly[2-(N,N-dimethyl amino) ethyl methacrylate] with dodecyl group (PDMAEMA-C12H25) was synthesized via the reversible addition-fragmentation chain transfer (RAFT) free radical polymerization with 2-{[(dodecy-sulfenyl)-carbonothionyl]sulfanyl} succinic acid (DCTSS) as chain transfer agent and AIBN as initiator.The effects of some parameters on the polymerization of DMAEMA were investigated,such as temperature,molar ratio of the chain transfer agent to the initiator.The structures and molecular weight of the products were characterized by 1HNMR and GPC.Meanwhile,surface properties of the product were measure.Results showed that at the reaction temperature of 70 ℃ and the molar ratio of the chain transfer agent to the initiator of 4:1,the molecular weight distribution of PDMAEMA-C12H25 is narrow and the reaction is controllable.The product displays rather lower critical micelle concentration (0.022 g·L-1) with lowest surface tension of 33.8 mN·m-1 (at 25 ℃),and good dispersing action for dyestuffs.
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    Lecture of science and technology
    Performance and applications of surfactants (Ⅺ) Foaming action of surfactant and its applications
    LIU Yuan-fei, HU Jun, ZHAO Li, XU Bao-cai, HAN Fu
    2014, 44 (11):  605-610.  doi: 10.13218/j.cnki.csdc.2014.11.135
    Abstract ( 286 )   PDF (825KB) ( 582 )  
    Structure and properties of foam were briefed.Actions of surfactant in formation,stabilization and breaking of foam were discussed.Foaming performance of surfactant and methods for its evaluation were described.Finally,applications of foaming performance of surfactant in fields of flotation separation,oil-field exploitation and fire extinguishment were summarized as well as its future development was prospected.
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    Development and application
    Synthesis and surface activity of the ester group trimethoxy organosilicon quaternary ammonium salt
    CHEN Rui-lan, ZHANG Jun-jie, MAO Tao-yan, ZHENG Cheng
    2014, 44 (11):  611-614.  doi: 10.13218/j.cnki.csdc.2014.11.136
    Abstract ( 244 )   PDF (795KB) ( 317 )  
    An ester group trimethoxy organosilicon quaternary ammonium salt was synthesized with stearic acid,dimethylethanolamine (DMEA) and γ-chloropropyl trimethoxy siloxane as starting materials.Structure of the product was characterized by FTIR,ESI-MS and 1HNMR,and the characterization results showed that the product is accord with the target.Via orthogonal designed experiments,the optimum reaction conditions for preparing the intermediate stearic acid dimethylethanolamine ester were obtained as:reaction temperature,180 ℃;reaction time,8 h;mole ratio,n(stearic acid):n(DMEA)=1:1.6;dosage of the catalyst,0.5%;and for the quaternarization,reaction temperature,110 ℃ under nitrogen atmosphere;mole ratio,n(stearic acid dimethylethanolamine ester):n(γ-chloropropyl trimethoxy siloxane)=1:1.4;dosage of the catalyst,0.5%;reaction time,28 h.The cmc of the product under 298 K were determined by steady-state fluorescence analysis as 0.009 3 g·L-1.
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    Preparation and performance of hair dye based upon hydroxyethyl-p-phenylenediamine sulfate
    YUE Juan, GAO Hai-yan, XU Yu, CHEN Qin-jun
    2014, 44 (11):  615-619.  doi: 10.13218/j.cnki.csdc.2014.11.137
    Abstract ( 684 )   PDF (1235KB) ( 357 )  
    Hydroxyethyl-p-phenylenediamine sulfate was used as dye intermediate to prepare hair dye.Meanwhile,the dyeing operating conditions were optimized.On this basis,a series of performance test for the dyed samples were conducted,and the results showed that,hydroxyethyl-p-phenylenediamine sulfate displays good oxidation resistance;and under conditions as pH 9,temperature 40 ℃ and time 20 min,the dye depth is biggest with comparatively less hair damage.At the same time,the results were compared with that of conventional hair dye based upon p-phenylenediamine,and it showed that the hair damage caused by hydroxyethyl-p-phenylenediamine sulfate is smaller and the hair retains good structural integrity under the same conditions.Furthermore,the dyed hair exhibits good UV-resistance.
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    Preparation and stability study of a lightening emulsion
    SHU Peng, KONG Sheng-zhong, GONG Sheng-zhao
    2014, 44 (11):  620-623.  doi: 10.13218/j.cnki.csdc.2014.11.138
    Abstract ( 365 )   PDF (771KB) ( 521 )  
    Stability of an emulsion system composed of undecylenoyl phenylalanine and phenylethyl resorcinol was studied.Main factors that affect stability of the emulsion,such as kinds and dosage of the emulsifying agent,emulsifying agent solubility in oil,selection of the thickening agent system,control of the emulsification homogenizer operating parameters et al.were investigated.Then the formulation and operating conditions for the preparation of the stable emulsion were identified as follows:composition (mass fraction) of emulsifying agant,2.00% of PEG-20 methyl glucose sesquistearate,1.00% of methyl glucose sesquistearate and 0.30% of sodium stearoyl glutamate (1.50% of potassium cetyl alcohol phosphate);composition (mass fraction) of oil phase,3.00% of ethylhexyl methoxycinnamate and 7.00% of octyldodecanol;composition (mass fraction) of thickening agents,2.00% of stearic acid,0.40% of hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer and 0.10% of xanthan gum;emulsification temperature,85 ℃;homogenizer speed,9 000 r·min-1.
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    Cloud point extraction technology of antioxidizing components from Nigella glandulifera seed meal
    LIU Xue, CAO Ying-can, HAN Wang-kang, YANG Cheng, CAO Guang-qun
    2014, 44 (11):  624-627.  doi: 10.13218/j.cnki.csdc.2014.11.139
    Abstract ( 214 )   PDF (786KB) ( 336 )  
    Cloud point extraction (CPE) was applied for the extraction of antioxidizing components from Nigella glandulifera seed meal (NGSM).The extraction technology was optimized by single factor experiment and orthogonally designed experiment with scavenging ratio of free radical of 1,1-diphenyl-2-trinitro-phenyl hydrazine (DPPH) as indicator for antioxidizing activity of the extract.The optimum extraction conditions were obtained as follows:surfactant mass concentration,40 g·L-1;liquid-solid ratio,35:1;ion strength,0.513 mol·L-1;and equilibration time,50 min.Under such conditions,the average DPPH free radical scavenging ratio achieves 86.87%,and the efficacy is related to its dosage.
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    Study on affecting factors of microbiological inspection of cosmetics
    XIE Xiao-bao, YANG Xiu-jiang, SUN Ting-li, LI Cai-ling, WEN Xia
    2014, 44 (11):  628-630.  doi: 10.13218/j.cnki.csdc.2014.11.140
    Abstract ( 301 )   PDF (1290KB) ( 369 )  
    Via setting up of two experimental groups,in which one composed of neutralizing agent and another without it,microbial inspection was carried out according to plate culture method that specified in China Hygienic Standard for Cosmetics.Experimental results on the colony detection of the two groups were compared.In the group with neutrazing agent added,10-fold dilution of cosmetics can be detected colonies,while in the group without neutralizing agent added,100-fold dilution of 18 cosmetics can be detected colonies,and 1 000-fold dilution of 2 creams can be detected colonies.Such results showed that the neutralizing agent can reduce the dilution of cosmetics when detection.Further,it was also found that TTC (2,3,5-triphenyl terazolium chloride) can inhibit the growth of bacteria in the cosmetics,so that TTC will affect the accuracy of the test results.It is recommended that verification test should be incorporated in the test standard;neutralizing agent should be added in the diluted solution of the cosmetics to reduce concentration of TTC in the culture medium;and 70% recovery of the test bacteria should be taken as the criteria for determining validity of the test.
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    Preparation and controlled releasing behavior of pH-sensitive konjac glucomannan complex gel
    XU Dong-ying, WANG Ying, MENG Ju-guang, LIN Shao-bin
    2014, 44 (11):  631-634.  doi: 10.13218/j.cnki.csdc.2014.11.141
    Abstract ( 300 )   PDF (1315KB) ( 347 )  
    Mixed polysaccharide of konjac glucomannan (KGM) and xanthan gum (XG) was used as the carrier and then β-cyclodextrin (β-CD) was further blended with the carrier to obtain KGM/XG/β-CD complex dry gel.Then vanillin was used as model flavor to prepare flavor loaded complex gel.Controlled releasing behavior of the flavor loaded complex gel was investigated and the results were compared with that of KGM/XG complex gel.Results showed that in buffered solutions of separate pH of 5,7 and 9 and after 12 h,the cumulative content of vanillin released from the KGM/XG complex gel reaches 45.0%,69.3% and 82.3% respectively;while that from the KGM/XG/β-CD complex gel reaches 29.5%,47.7% and 60.6%,respectively,which are significantly lower.Such results indicated that the cavity structure of β-CD provides a controlled releasing effect on vanillin.
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    Technology for two-step synthesis of aroma chemical dynascone
    MA Hong-liang, LI Rui, WU Qi-lin, JIANG Xing-tao
    2014, 44 (11):  635-637.  doi: 10.13218/j.cnki.csdc.2014.11.142
    Abstract ( 427 )   PDF (746KB) ( 407 )  
    Firstly 1-acetyl-5,5-dimethyl-1-cyclohexene was obtained via rearrangement cyclization reaction with dehydrolinalool as starting material and poly-phosphoric acid (PPA) as catalyst,and then via the alkylation reaction to synthesize the targeted product dynascone.The overall yield of the two steps achieves 40.8%.The product was characterized by IR,1HNMR,13CNMR and GC-MS.Effect of dosage of the catalyst,reaction temperature and catalyst reusing on yield of 1-acetyl-5,5-dimethyl-1-cyclohexene was investigated.Results showed that yield of 1-acetyl-5,5-dimethyl-1-cyclohexene achieves 97.0% based on 80 ℃ of reaction temperature and mass ratio of dehydrolinalool to PPA 1:2.The catalyst PPA can be reused for 2~3 times.
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    Reviews
    Progress in research work with respect to hydrocarbon/fluorocarbon hybrid surfactants
    YANG Mei, HAO Jing-cheng, LI Hong-guang
    2014, 44 (11):  638-643.  doi: 10.13218/j.cnki.csdc.2014.11.143
    Abstract ( 217 )   PDF (2800KB) ( 296 )  
    Basic conception for hydrocarbon/fluorocarbon hybrid surfactants where both a hydrocarbon chain and a fluorocarbon chain are integrated into the same surfactant molecule was introduced.Their development history,research work status and synthesis method for typical molecules were described.Their rheological characteristics,aggregation behavior and practical applications in fields of emulsification and biomedicine were summarized.It was put forward that the development of new generation of hydrocarbon/fluorocarbon hybrid surfactants should be orientatively proceeded from molecular structure design.
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    Progress in field of research work with respect to synthesis and applications of Gemini surfactants
    GAO Nan, LI Guo-rong, CHEN Xu-dong
    2014, 44 (11):  644-651.  doi: 10.13218/j.cnki.csdc.2014.11.144
    Abstract ( 511 )   PDF (947KB) ( 931 )  
    The recent domestic and international progress in field of research and development work with respect to syntheses,properties and applications of functional Gemini surfactants were reviewed.Main synthesis methods and performances of ionic,nonionic,amphoteric and asymmetric Gemini surfactants were described.Applications of Gemini surfactants in daily use chemicals,emulsion polymerization,metal corrosion prevention,biotechnology and tertiary oil recovery were discussed as well.Furthermore,the prospective future of Gemini surfactants was also prognosticated.
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    Analytical methods and testing
    Determination of nitroimidazoles in acne dispelling cosmetics with solid phase extraction and high performance liquid chromatography-tandem mass spectrometry
    LU Jian, WU Zhong-ping, CHE Wen-jun, HONG Hua, YANG Yang
    2014, 44 (11):  652-655.  doi: 10.13218/j.cnki.csdc.2014.11.145
    Abstract ( 225 )   PDF (868KB) ( 407 )  
    A method for simultaneous determination of six kinds of nitroimidazole drug (metronidazole (MNZ),tinidazole (TNZ),ornidazole (ONZ),dimetridazole (DMZ),ronidazole (RNZ) and secnidazole (SCZ)) in acne dispelling cosmetics adopting solid phase extraction (SPE) purification technology and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was studied and established.Samples were extracted with acidified acetonitrile solution and the extract was purified with cation resin solid phase exchanging column.Then the purified extract was separated with a C18 column,by gradient elution with acetonitrile and water (containing 0.1% formic acid,volume fraction),and detected by tandem mass spectrometry under multiple reaction monitoring (MRM) mode.The results indicated that good linearity displays when mass concentration of the six kinds of nitroimidazole is within 1.0~50.0 μg·L-1,and all the linear correlation coefficients are higher than 0.999.All the limits of quantification (LOQ) are 0.5 mg·kg-1.The recoveries of six kinds of nitroimidazole when three levels of standard were spiked into samples of acne dispelling cosmetics (both cream type and lotion type) range from 89.7% to 108.0% with RSD (n=6) from 2.3% to 6.5%.
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    Monitoring of dehydration reaction in the production process of L-pyroglutamic acid by HPLC
    YE Ai-ying, XU Jin, ZHANG Wen-wen, WU Fang-zhen
    2014, 44 (11):  656-658.  doi: 10.13218/j.cnki.csdc.2014.11.146
    Abstract ( 351 )   PDF (728KB) ( 288 )  
    HPLC was applied to monitor the dehydration reaction,in the production process of L-pyroglutamic acid from L-glutamic acid.The chromatography is operated by adopting a YMC-Pack Pro C18 RP column (4.6 mm×250 mm×5 μm) and mobile phase composed of aqueous solution of 5 mmol·L-1 potassium dihydro phosphate and 0.05 mmol·L-1 ammonium dihydro phosphate in combination of acetonitrile with volume ratio of 9:1.The content of L-pyroglutamic acid in reaction solution was determined by the standard spiking method.The results showed that the plot of the content and the peak area displays good linearity in the range of 0.017 8~0.065 3 g·L-1 with r=0.998 7;the average recovery is 99.31%,while the relative standard deviation for repetitions is 0.45%.Based upon this monitoring method,it showed that the dehydration reaction achieves the best condition at reaction time of 1 h.
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