A fluorine-containing polyacrylate copolymer emulsion was synthesized by a seed emulsion polymerization method, in which methyl methacrylate （MMA） and butyl acrylate （BA） were used as main monomers and hexafluorob...A fluorine-containing polyacrylate copolymer emulsion was synthesized by a seed emulsion polymerization method, in which methyl methacrylate （MMA） and butyl acrylate （BA） were used as main monomers and hexafluorobutyl methacrylate （HFMA） as fluorine-containing monomer. The structure and properties were characterized by Fourier transform infrared spectrum （FT-IR）, transmission electron microscopy （TEM）, particle size analysis, X-ray photoelectron spectroscopy （XPS）, contact angle （CA）, differential scanning calorimetry （DSC） and thermogravimetry （TG） analysis. The FTIR and TEM results showed that HFMA was effectively involved in the emulsion copolymerization, and the formed emulsion particles had a core-shell structure and a narrow particle size distribution. XPS and CA analysis revealed that a gradient concentration of fluorine existed in the depth profile of fluorine-containing emulsion film which was richer in fluorine and more hydrophobic in one side. DSC and TG analysis also showed that a clear core-shell structure existed in the fluorine-containing emulsion particles, and their film showed higher thermal stability than that of fluorine-free emulsion.展开更多
A series of novel fluorine-containing acrylates 6a-6g were synthesized via the condensation of ethyl cyanoacetate and trifluoroacetic anhydride, followed by chloridization and the coupling reaction with amines. These ...A series of novel fluorine-containing acrylates 6a-6g were synthesized via the condensation of ethyl cyanoacetate and trifluoroacetic anhydride, followed by chloridization and the coupling reaction with amines. These new compounds exhibited some biological activity as preliminary bioassay indicated. A plausible reaction mechanism was outlined and discussed.展开更多
The inhibiting effect of ciprofloxacin,norfloxacin and ofloxacin on the corrosion of mild steel in 1 mol·L-1 HCl and the mechanism were studied at different temperatures using mass loss measurement,electrochemica...The inhibiting effect of ciprofloxacin,norfloxacin and ofloxacin on the corrosion of mild steel in 1 mol·L-1 HCl and the mechanism were studied at different temperatures using mass loss measurement,electrochemical method,and X-ray photoelectron spectroscopy(XPS) .Effective inhibition was shown by mass loss,potentiodynamic polarization and impedance spectroscopy measurement.The corrosion rate of the metal in the mass loss measurement,and the corrosion reaction on cathode and anode in the electrochemical measurement were accelerated when temperature was increased.XPS results showed that the inhibitors adsorbed effectively on the metal surface.展开更多
Polymer coated quartz crystal microbalance (QCM) sensor based on the frequency shifts due to the adsorption of compounds at the surface of modified quartz crystal electrode is an effective method for detection of sari...Polymer coated quartz crystal microbalance (QCM) sensor based on the frequency shifts due to the adsorption of compounds at the surface of modified quartz crystal electrode is an effective method for detection of sarin (GB) which is a highly toxic nerve warfare agent. A new fluorosiloxane polymer has been synthesized through 6 steps from trifluoromethyl benzene. The synthesis was achieved from trifluoromethyl benzene through nitration, hydrogenation. The obtained m-nitrotrifluoromethyl aniline was treated with NaNO2, and then hydrolyzed to m-nitrotrifluoromethyl phenol. m-nitrotrifluoromethyl phenol was reacted with allyl bromide to the ether product. The product was rearranged by Claisen rearrangement, and then reacted with polymethylhydrosiloxane under catalyst of Pt/DVTMS. The fluorosiloxane polymer can be obtained. The polymer has been successfully used as QCM coating material.展开更多
Objective:To observe the effect of warm-unblocking acupuncture plus fluticasone propionate nasal spray on the pulmonary ventilation,level of interferon-y(IFN-y)and sleep quality in parents with allergic rhinitis(AR).M...Objective:To observe the effect of warm-unblocking acupuncture plus fluticasone propionate nasal spray on the pulmonary ventilation,level of interferon-y(IFN-y)and sleep quality in parents with allergic rhinitis(AR).Methods:A total of 112 AR patients were enrolled between January 2013 and August 2018 and were divided into an observation group and a control group by the random number table method,with 56 cases in each group.Patients in the observation group received warm-unblocking acupuncture plus fluticasone propionate nasal spray,and patients in the control group only received fluticasone propionate nasal spray.The nasal symptom score,pulmonary function indexes,the levels of IFN-y and interleukin(IL)-4 in serum,and sleep quality in the two groups were compared.Results:After treatment,the total effective rate in the observation group was higher than that in the control group(P<0.05).The nasal symptom score dropped in both groups after treatment(both P<0.05),and the score in the observation group was lower than that in the con trol group(P<0.05).The pulm onary ven tilati on indexes all in creased sign ificantly after treatment in the observation group(all P<0.05);the forced expiratory volume in 1 second(FEV1)to forced vital capacity(FVC)ratio(FEV1/FVC)and the forced expiratory flow at 50%,75%and 25%-75%of the vital capacity(FEF50%,FEF75%,FEF25%-75%)in creased after treatme nt in the control group(all P<0.05);the pulm onary ven tilati on in dexes were higher in the observati on group tha n those in the control group(all P<0.05).The level of IFN-y in creased sign ificantly after t reatment in the two groups(both P<0.05)and the level of IL-4 dropped significantly(both P<0.05);the observation group had a higher IFN-y level(P<0.05)and a lower IL-4 level(P<0.05)compared with the control group.Regarding the Pittsburgh sleep quality index(PSQI),the scores of subjective sleep quality,habitual sleep efficiency and sleep disturbances and the general PSQI score decreased significantly after treatment in both groups(all P<0.05),and the scores in the observation group were significantly lower than those in the control group(all P<0.05).Conclusion:Warm-unblocking acupuncture plus fluticasone propionate nasal spray can effectively control the clinical symptoms and improve pulmonary function in the treatment of AR;this approach can regulate the levels of IFN-y and IL-4 towards the normal range in AR patients;it can also improve patient's sleep quality.This method can produce more significant efficacy than fluticasone propionate nasal spray used alone.展开更多
Combined administration of fluticasone propionate and salmeterol xinofoate has been widely used for the treatment of asthma in recent decades. In this investigation, we developed and validated a novel and sensitive ul...Combined administration of fluticasone propionate and salmeterol xinofoate has been widely used for the treatment of asthma in recent decades. In this investigation, we developed and validated a novel and sensitive ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） method for simultaneous determination of fluticasone propionate and salmeterol xinofoate in human plasma. Following a simple SPE sample extraction in 96-well plate format, chromatography was performed on a Waters ACQUITY UPLC BEH C 18 column （1.7 μm, 50 min×2.1 mm） with mobile phase consisting of 100% MeOH and 0.1% NH4OH in water on a gradient program at flow rate of 0.5 mL/min. Detection of analytes and internal standards was accomplished using multiple reaction monitoring （MRM） of precursor〉product ion pairs of m/z 501.4〉313.2 （fluticasone propionate）, 506.4〉293.3 （fluticasone propionate-d5）, 416.4〉232.1 （salmeterol xinofoate） and 419.3〉235.2 （salmeterol-d3）. The assay range was 2.50-500 pg/mL for both analytes, and a 1/x2 weighted linear regression model was used. The inter-assay accuracy and precision of the method were within ±8.6%. The recoveries from 0.30 mL of plasma were greater than 51.0% and 54.6% for fluticasone propionate and salmeterol, respectively, and the results were consistent across low, middle and high concentration levels. The method was validated following FDA, EMA and CFDA （China Food and Drug Administration）＇s guidance on bioanalysis and then successfully applied to support a clinical study in healthy Chinese subjects following inhaled administration of a single combination of fluticasone propionate/salmeterol （250 μg/50 μg）.展开更多
Synthesis and anionic polymerization of the fluorine-substituted phenyl methacrylates are herein reported. A series of monodi-, and multi-substituted fluorophenyl methacrylates H2C=C（CH3）C（O）OC6H4F-4 （M^1a）, H2...Synthesis and anionic polymerization of the fluorine-substituted phenyl methacrylates are herein reported. A series of monodi-, and multi-substituted fluorophenyl methacrylates H2C=C（CH3）C（O）OC6H4F-4 （M^1a）, H2C=C（CH3）C（O）OC6H4F-3 （M^1b）, HEC=C（CH3）C（O）OC6H3F2-2,4 （M^2）, H2C=C（CH3）C（O）OC6H2F3-2,3,4 （M^3）, H2C=C（CH3）C（O）OC6HF4-2,3,5,6 （M^4）, and H2C=C（CH3）C（O）OC6F5 （M^5） were synthesized and characterized. Initially, the polymerization was carded out on the monomer M^1a by using nBuLi, tBuLi, and KH as the respective catalysts; this approach produced the polymers in yields of 12%-50%, but with lower molecular weights. Similar results were obtained by using tBuLi for catalytically polymerizing the other five monomers. By introducing a co-catalyst MeAl（BHT）2, the catalysts Nail, LiH, and tBuOLi each were tested to polymerize M^1a, which gave the polymers in very low yields （3%-7%）. Polymer yields of 13%-27% were obtained by each of the catalysts LiAlH4, nBuLi, PhLi, and tBuLi in connection with MeAI（BHT）2, but a better yield （61%） was achieved with KH/MeAl（BHT）2. The KH/MeAl（BHT）2 catalyst system was further employed to polymerize M^1b and M^2, which afforded respective polymer yields of 12%-63% and 10%-53%, depending on the molar ratios of KH：MeAl（BHT）2 as well as on the monomer concentrations. All of the polymers produced were syndiotactically rich in structure, as indicated by either ^1H or ^19F NMR data. The polymerization mechanism by the combined catalyst system is proposed.展开更多
基金Supported by the National Natural Science Foundation of China （20476035, 20846003）.
文摘A fluorine-containing polyacrylate copolymer emulsion was synthesized by a seed emulsion polymerization method, in which methyl methacrylate （MMA） and butyl acrylate （BA） were used as main monomers and hexafluorobutyl methacrylate （HFMA） as fluorine-containing monomer. The structure and properties were characterized by Fourier transform infrared spectrum （FT-IR）, transmission electron microscopy （TEM）, particle size analysis, X-ray photoelectron spectroscopy （XPS）, contact angle （CA）, differential scanning calorimetry （DSC） and thermogravimetry （TG） analysis. The FTIR and TEM results showed that HFMA was effectively involved in the emulsion copolymerization, and the formed emulsion particles had a core-shell structure and a narrow particle size distribution. XPS and CA analysis revealed that a gradient concentration of fluorine existed in the depth profile of fluorine-containing emulsion film which was richer in fluorine and more hydrophobic in one side. DSC and TG analysis also showed that a clear core-shell structure existed in the fluorine-containing emulsion particles, and their film showed higher thermal stability than that of fluorine-free emulsion.
基金The project supported by the National Natural Science Foundation of China(No.2017203 1)the Chinese Research Fund for the Doctoral Pr ogram of High Education.
文摘A series of novel fluorine-containing acrylates 6a-6g were synthesized via the condensation of ethyl cyanoacetate and trifluoroacetic anhydride, followed by chloridization and the coupling reaction with amines. These new compounds exhibited some biological activity as preliminary bioassay indicated. A plausible reaction mechanism was outlined and discussed.
基金Supported by the National Science ＆ Technology Pillar Program（082603101c） China Postdoctoral Science Foundation （O92623101H）+2 种基金 Shandong Postdoctoral Foundation（200902040） Open Project Program of Marine Corrosion and Protection Research Center of Institute of Oceanology Chinese Academy of Science（200901005） Doctor Foundation of University of Jinan（XBS0899）
文摘The inhibiting effect of ciprofloxacin,norfloxacin and ofloxacin on the corrosion of mild steel in 1 mol·L-1 HCl and the mechanism were studied at different temperatures using mass loss measurement,electrochemical method,and X-ray photoelectron spectroscopy(XPS) .Effective inhibition was shown by mass loss,potentiodynamic polarization and impedance spectroscopy measurement.The corrosion rate of the metal in the mass loss measurement,and the corrosion reaction on cathode and anode in the electrochemical measurement were accelerated when temperature was increased.XPS results showed that the inhibitors adsorbed effectively on the metal surface.
文摘Polymer coated quartz crystal microbalance (QCM) sensor based on the frequency shifts due to the adsorption of compounds at the surface of modified quartz crystal electrode is an effective method for detection of sarin (GB) which is a highly toxic nerve warfare agent. A new fluorosiloxane polymer has been synthesized through 6 steps from trifluoromethyl benzene. The synthesis was achieved from trifluoromethyl benzene through nitration, hydrogenation. The obtained m-nitrotrifluoromethyl aniline was treated with NaNO2, and then hydrolyzed to m-nitrotrifluoromethyl phenol. m-nitrotrifluoromethyl phenol was reacted with allyl bromide to the ether product. The product was rearranged by Claisen rearrangement, and then reacted with polymethylhydrosiloxane under catalyst of Pt/DVTMS. The fluorosiloxane polymer can be obtained. The polymer has been successfully used as QCM coating material.
文摘Objective:To observe the effect of warm-unblocking acupuncture plus fluticasone propionate nasal spray on the pulmonary ventilation,level of interferon-y(IFN-y)and sleep quality in parents with allergic rhinitis(AR).Methods:A total of 112 AR patients were enrolled between January 2013 and August 2018 and were divided into an observation group and a control group by the random number table method,with 56 cases in each group.Patients in the observation group received warm-unblocking acupuncture plus fluticasone propionate nasal spray,and patients in the control group only received fluticasone propionate nasal spray.The nasal symptom score,pulmonary function indexes,the levels of IFN-y and interleukin(IL)-4 in serum,and sleep quality in the two groups were compared.Results:After treatment,the total effective rate in the observation group was higher than that in the control group(P<0.05).The nasal symptom score dropped in both groups after treatment(both P<0.05),and the score in the observation group was lower than that in the con trol group(P<0.05).The pulm onary ven tilati on indexes all in creased sign ificantly after treatment in the observation group(all P<0.05);the forced expiratory volume in 1 second(FEV1)to forced vital capacity(FVC)ratio(FEV1/FVC)and the forced expiratory flow at 50%,75%and 25%-75%of the vital capacity(FEF50%,FEF75%,FEF25%-75%)in creased after treatme nt in the control group(all P<0.05);the pulm onary ven tilati on in dexes were higher in the observati on group tha n those in the control group(all P<0.05).The level of IFN-y in creased sign ificantly after t reatment in the two groups(both P<0.05)and the level of IL-4 dropped significantly(both P<0.05);the observation group had a higher IFN-y level(P<0.05)and a lower IL-4 level(P<0.05)compared with the control group.Regarding the Pittsburgh sleep quality index(PSQI),the scores of subjective sleep quality,habitual sleep efficiency and sleep disturbances and the general PSQI score decreased significantly after treatment in both groups(all P<0.05),and the scores in the observation group were significantly lower than those in the control group(all P<0.05).Conclusion:Warm-unblocking acupuncture plus fluticasone propionate nasal spray can effectively control the clinical symptoms and improve pulmonary function in the treatment of AR;this approach can regulate the levels of IFN-y and IL-4 towards the normal range in AR patients;it can also improve patient's sleep quality.This method can produce more significant efficacy than fluticasone propionate nasal spray used alone.
文摘Combined administration of fluticasone propionate and salmeterol xinofoate has been widely used for the treatment of asthma in recent decades. In this investigation, we developed and validated a novel and sensitive ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） method for simultaneous determination of fluticasone propionate and salmeterol xinofoate in human plasma. Following a simple SPE sample extraction in 96-well plate format, chromatography was performed on a Waters ACQUITY UPLC BEH C 18 column （1.7 μm, 50 min×2.1 mm） with mobile phase consisting of 100% MeOH and 0.1% NH4OH in water on a gradient program at flow rate of 0.5 mL/min. Detection of analytes and internal standards was accomplished using multiple reaction monitoring （MRM） of precursor〉product ion pairs of m/z 501.4〉313.2 （fluticasone propionate）, 506.4〉293.3 （fluticasone propionate-d5）, 416.4〉232.1 （salmeterol xinofoate） and 419.3〉235.2 （salmeterol-d3）. The assay range was 2.50-500 pg/mL for both analytes, and a 1/x2 weighted linear regression model was used. The inter-assay accuracy and precision of the method were within ±8.6%. The recoveries from 0.30 mL of plasma were greater than 51.0% and 54.6% for fluticasone propionate and salmeterol, respectively, and the results were consistent across low, middle and high concentration levels. The method was validated following FDA, EMA and CFDA （China Food and Drug Administration）＇s guidance on bioanalysis and then successfully applied to support a clinical study in healthy Chinese subjects following inhaled administration of a single combination of fluticasone propionate/salmeterol （250 μg/50 μg）.
基金supported by the National Basic Research Program of China(2012CB821704)the National Natural Science Foundation of China(20972129)the Innovative Research Team Program(IRT1036,J1310024)
文摘Synthesis and anionic polymerization of the fluorine-substituted phenyl methacrylates are herein reported. A series of monodi-, and multi-substituted fluorophenyl methacrylates H2C=C（CH3）C（O）OC6H4F-4 （M^1a）, H2C=C（CH3）C（O）OC6H4F-3 （M^1b）, HEC=C（CH3）C（O）OC6H3F2-2,4 （M^2）, H2C=C（CH3）C（O）OC6H2F3-2,3,4 （M^3）, H2C=C（CH3）C（O）OC6HF4-2,3,5,6 （M^4）, and H2C=C（CH3）C（O）OC6F5 （M^5） were synthesized and characterized. Initially, the polymerization was carded out on the monomer M^1a by using nBuLi, tBuLi, and KH as the respective catalysts; this approach produced the polymers in yields of 12%-50%, but with lower molecular weights. Similar results were obtained by using tBuLi for catalytically polymerizing the other five monomers. By introducing a co-catalyst MeAl（BHT）2, the catalysts Nail, LiH, and tBuOLi each were tested to polymerize M^1a, which gave the polymers in very low yields （3%-7%）. Polymer yields of 13%-27% were obtained by each of the catalysts LiAlH4, nBuLi, PhLi, and tBuLi in connection with MeAI（BHT）2, but a better yield （61%） was achieved with KH/MeAl（BHT）2. The KH/MeAl（BHT）2 catalyst system was further employed to polymerize M^1b and M^2, which afforded respective polymer yields of 12%-63% and 10%-53%, depending on the molar ratios of KH：MeAl（BHT）2 as well as on the monomer concentrations. All of the polymers produced were syndiotactically rich in structure, as indicated by either ^1H or ^19F NMR data. The polymerization mechanism by the combined catalyst system is proposed.
