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2015 Volume 32 Issue 2
2015, 32(2): 123-133
doi: 10.11944/j.issn.1000-0518.2015.02.140187
Abstract:
Dithiocarbamate compounds have become the focus of pharmaceutical chemistry in recent years due to their unique molecular structure with a variety of biological properties,such as anti-tumor,antibacterium, antioxidation and insecticidal activity. This article reviews recent progresses in the biological activities of dithiocarbamate compounds and gives prospects for their development and application.
Dithiocarbamate compounds have become the focus of pharmaceutical chemistry in recent years due to their unique molecular structure with a variety of biological properties,such as anti-tumor,antibacterium, antioxidation and insecticidal activity. This article reviews recent progresses in the biological activities of dithiocarbamate compounds and gives prospects for their development and application.
2015, 32(2): 134-142
doi: 10.11944/j.issn.1000-0518.2015.02.140114
Abstract:
Bio-electrochemical system provides a novel and low energy consumption process for seawater desalination. In this article,the updated research progress is reviewed since the invention of microbial desalination cell(MDC) in 2009. The principle of MDC and the evaluating parameters of the system are briefly introduced. The desalination performance in different integration of MDC with traditional desalination technologies is compared. The existing problems and limiting factors for the practical utilization are discussed. And the challenges and perspective are stated.
Bio-electrochemical system provides a novel and low energy consumption process for seawater desalination. In this article,the updated research progress is reviewed since the invention of microbial desalination cell(MDC) in 2009. The principle of MDC and the evaluating parameters of the system are briefly introduced. The desalination performance in different integration of MDC with traditional desalination technologies is compared. The existing problems and limiting factors for the practical utilization are discussed. And the challenges and perspective are stated.
2015, 32(2): 143-150
doi: 10.11944/j.issn.1000-0518.2015.02.140191
Abstract:
A series of 2,3-disubstituted-1,3-benzoxazines was synthesized by trimethyl chlorosilane-catalyzed aza-acetalization of 2-arylaminomethyl phenols with aromatic aldehydes. The structures of the prepared compounds were characterized by FT-IR,1H NMR,13C NMR and elemental analysis. Fungicidal activities of these compounds were also evaluated. Most of them exhibit good activities. Compound 6e shows 79% and 77.9% activity against S. Scleratotiorum and B. Cinérea,respectively. Compounds 6a and 6d exhibit 74.8% activity against S. Scleratotiorum.
A series of 2,3-disubstituted-1,3-benzoxazines was synthesized by trimethyl chlorosilane-catalyzed aza-acetalization of 2-arylaminomethyl phenols with aromatic aldehydes. The structures of the prepared compounds were characterized by FT-IR,1H NMR,13C NMR and elemental analysis. Fungicidal activities of these compounds were also evaluated. Most of them exhibit good activities. Compound 6e shows 79% and 77.9% activity against S. Scleratotiorum and B. Cinérea,respectively. Compounds 6a and 6d exhibit 74.8% activity against S. Scleratotiorum.
2015, 32(2): 151-157
doi: 10.11944/j.issn.1000-0518.2015.02.140163
Abstract:
A series of 4-(1-phenyl-3-methyl-5-chloro-1H-pyrazolelideneamino)-5-(substituted aryl)-2H-1,2,4-triazole-3(4H)-thiones was synthesized by the condensation reaction of 5-chloro-1-phenyl-3-methyl-1Hpyrazole-4-aldehyde with 4-amino-5-(substituted phenyl-2H-1,2,4-triazole-3(4H)-thione. Alkylation of compound 6 with ethyl-2-chloroacetate or 1-(chloromethyl)-4-nitrobenzene afforded 5,6-2H-[1,2,4] triazolo[3,4-b] [1,3,4]thiadiazine derivatives containing pyrazole unit. Their structures were confirmed by 1H NMR,IR and elemental analyses. Preliminary bioassay indicates that the anti-fungicidal activity of compound 8a (3-(2-methyphenyl)-6-(5-chloro-2-methyl-4-phenylpyrazole)-7-(4-nitrophenyl)-5H-1,2,4-triazolo[3,4-b] [1,3,4]thiadiazine) to Colletotrichum lagenarium at the concentration of 100 mg/L is 90%.
A series of 4-(1-phenyl-3-methyl-5-chloro-1H-pyrazolelideneamino)-5-(substituted aryl)-2H-1,2,4-triazole-3(4H)-thiones was synthesized by the condensation reaction of 5-chloro-1-phenyl-3-methyl-1Hpyrazole-4-aldehyde with 4-amino-5-(substituted phenyl-2H-1,2,4-triazole-3(4H)-thione. Alkylation of compound 6 with ethyl-2-chloroacetate or 1-(chloromethyl)-4-nitrobenzene afforded 5,6-2H-[1,2,4] triazolo[3,4-b] [1,3,4]thiadiazine derivatives containing pyrazole unit. Their structures were confirmed by 1H NMR,IR and elemental analyses. Preliminary bioassay indicates that the anti-fungicidal activity of compound 8a (3-(2-methyphenyl)-6-(5-chloro-2-methyl-4-phenylpyrazole)-7-(4-nitrophenyl)-5H-1,2,4-triazolo[3,4-b] [1,3,4]thiadiazine) to Colletotrichum lagenarium at the concentration of 100 mg/L is 90%.
2015, 32(2): 158-165
doi: 10.11944/j.issn.1000-0518.2015.02.140151
Abstract:
Based on the piecing together principle in the drug design,we directly couple the hydroxyl group of lead compounds with bioactive compounds in order to get hydroquinone derivatives with high efficiency and low toxicity. 4-(Benzyloxy) phenol was synthesized through the protection of phenolic hydroxyl group,and then coupled with amino acid whose amino group was protected. Moreover,we introduced carboxylic acid moeity into 4-(benzyloxy) phenol and coupled it with amino acid methyl ester hydrochloride. After the removal of the benzyl protecting group,sixteen amino acid-hydroquinone conjugates were synthesized. The sixteen conjugates were characterized by IR,1H NMR,13C NMR and ESI-MS. The study of whitening activity of these conjugates showed that HQ-3b,HQ-3c,HQ-4a,HQ-4b,HQ-7c and HQ-8a had significant inhibition to tyrosinase(IC50=3.60) with the IC50 of HQ-4b as low as 0.15.
Based on the piecing together principle in the drug design,we directly couple the hydroxyl group of lead compounds with bioactive compounds in order to get hydroquinone derivatives with high efficiency and low toxicity. 4-(Benzyloxy) phenol was synthesized through the protection of phenolic hydroxyl group,and then coupled with amino acid whose amino group was protected. Moreover,we introduced carboxylic acid moeity into 4-(benzyloxy) phenol and coupled it with amino acid methyl ester hydrochloride. After the removal of the benzyl protecting group,sixteen amino acid-hydroquinone conjugates were synthesized. The sixteen conjugates were characterized by IR,1H NMR,13C NMR and ESI-MS. The study of whitening activity of these conjugates showed that HQ-3b,HQ-3c,HQ-4a,HQ-4b,HQ-7c and HQ-8a had significant inhibition to tyrosinase(IC50=3.60) with the IC50 of HQ-4b as low as 0.15.
2015, 32(2): 166-170
doi: 10.11944/j.issn.1000-0518.2015.02.140125
Abstract:
High purity 2,6-dihydroxynaphthalene was synthesized by one-pot alkali fusion using cheap disodium 2,6-naphthalenedisulfonate as the starting material. Under nitrogen atmosphere,in order to avoid overoxidation and obtain high yield of 2,6-dihydroxynaphthalene,phenol or antioxidant 1010 was added. Under the optimal technological conditions,the mass ratio of disodium 2,6-naphthalenedisulfonate and alkali 1:3,the mass ratio of sodium hydroxide and potassium hydroxide 2:1 in mixed alkali,the reaction temperature 345℃,the yield of 2,6-dihydroxynaphthalene in the alkali fusion is 86.3%. It is confirmed that the purity of 2,6-dihydroxynaphthalene is up to 99% after being refined by a methanol-water mixed solvent.
High purity 2,6-dihydroxynaphthalene was synthesized by one-pot alkali fusion using cheap disodium 2,6-naphthalenedisulfonate as the starting material. Under nitrogen atmosphere,in order to avoid overoxidation and obtain high yield of 2,6-dihydroxynaphthalene,phenol or antioxidant 1010 was added. Under the optimal technological conditions,the mass ratio of disodium 2,6-naphthalenedisulfonate and alkali 1:3,the mass ratio of sodium hydroxide and potassium hydroxide 2:1 in mixed alkali,the reaction temperature 345℃,the yield of 2,6-dihydroxynaphthalene in the alkali fusion is 86.3%. It is confirmed that the purity of 2,6-dihydroxynaphthalene is up to 99% after being refined by a methanol-water mixed solvent.
2015, 32(2): 171-176
doi: 10.11944/j.issn.1000-0518.2015.02.140140
Abstract:
A benzo-15-crown-5 modified 5-(4-carboxyphenyl)-10,15,20-triphenylporphyrin (1) was synthesized and used for binding with Hg2+ ion to form crown ether metal-prophyrin complex(3). UV-Vis and 1H NMR were used to investigate the formation and self-assembly of complex 3. The difference of 1H NMR spectra of complexes 3 and 2 reveals that a synergy effect of prophyrin and crown ether exists. The anion recognition and mechanism of complex 3 were also studied. After addition of NaNH2,an obvious red shift in the UV-Vis spectra was observed accompanied with a color change from green to chartreuse viewed by naked eye. At the same time,the chemical shift of -CH2- in crown ether ring shifted from 3.12 to 3.16 and 3.32 to 3.34,respectively. This phenomenon can be explained by the strong nucleophilic property of amino anion. However,addition of other sodium salts such as NaCl,NaH2PO4 and NaHCO3 could not result in the same phenomenon. This study provides a method for visible anion recognition.
A benzo-15-crown-5 modified 5-(4-carboxyphenyl)-10,15,20-triphenylporphyrin (1) was synthesized and used for binding with Hg2+ ion to form crown ether metal-prophyrin complex(3). UV-Vis and 1H NMR were used to investigate the formation and self-assembly of complex 3. The difference of 1H NMR spectra of complexes 3 and 2 reveals that a synergy effect of prophyrin and crown ether exists. The anion recognition and mechanism of complex 3 were also studied. After addition of NaNH2,an obvious red shift in the UV-Vis spectra was observed accompanied with a color change from green to chartreuse viewed by naked eye. At the same time,the chemical shift of -CH2- in crown ether ring shifted from 3.12 to 3.16 and 3.32 to 3.34,respectively. This phenomenon can be explained by the strong nucleophilic property of amino anion. However,addition of other sodium salts such as NaCl,NaH2PO4 and NaHCO3 could not result in the same phenomenon. This study provides a method for visible anion recognition.
2015, 32(2): 177-182
doi: 10.11944/j.issn.1000-0518.2015.02.140164
Abstract:
9,10-Bis ((4-(2-(2-(2-methoxyethoxy) ethoxy) ethoxy) phenyl) ethynyl) anthracene (1) was synthesized by Sonogashira coupling. Its structure was characterized by 1H NMR and MALDI-TOF mass spectroscopy. The self-assembling behavior of compound 1 was investigated by means of differential scanning calorimetry(DSC),thermal polarized optical microscopy(POM),and small-angle X-ray scattering(SAXS) at the bulk state. Compound 1 self-assembled into smectic A phase (SmA) in the solid state. Spectroscopic analysis suggested that compound 1 inherited the characteristic of high fluorescence quantum yield (Φf) of disubstituted anthracenes. The title compound 1 is a kind of photoluminescence materials with good performance.
9,10-Bis ((4-(2-(2-(2-methoxyethoxy) ethoxy) ethoxy) phenyl) ethynyl) anthracene (1) was synthesized by Sonogashira coupling. Its structure was characterized by 1H NMR and MALDI-TOF mass spectroscopy. The self-assembling behavior of compound 1 was investigated by means of differential scanning calorimetry(DSC),thermal polarized optical microscopy(POM),and small-angle X-ray scattering(SAXS) at the bulk state. Compound 1 self-assembled into smectic A phase (SmA) in the solid state. Spectroscopic analysis suggested that compound 1 inherited the characteristic of high fluorescence quantum yield (Φf) of disubstituted anthracenes. The title compound 1 is a kind of photoluminescence materials with good performance.
2015, 32(2): 183-191
doi: 10.11944/j.issn.1000-0518.2015.02.140176
Abstract:
Chloromethylated Polystyrene (CMPS) was first prepared with 1,4-bis (chloromethoxy) butane (BCMB) as the chloromethylation reagent. Then nucleophilic substitution between CMPS and phydroxybenzaldehyde(HBA) was conducted,resulting in benzaldehyde(BA) modified polystyrene(PS-BA) on its side chain. Finally,a reaction between 3-aminopyridine(AP) and the aldehyde group of PS-BA was allowed to form Schiff base functionalized polystyrene PS-SB. The chemical structure of PS-SB was characterized by FTIR and 1H NMR spectra. PS-SB as the first ligand and phenanthroline (Phen) as the second ligand,binary and ternary polymer-rare earth complexes,PS-(SB)3-Eu(Ⅲ) and PS-(SB)3-Eu(Ⅲ)-(Phen),were prepared,respectively. The florescence emission properties of the two complexes were preliminarily explored. The experimental results show that the rate of the nucleophilic substitution reaction between CMPS and HBA has a mechanism of SN 1. For the nucleophilic substitution reaction,N,Ndimethylacetamide(DMAC) with stronger polarity is a suitable solvent,and the temperature of 80℃ is appropriate. The macromolecular ligand PS-SB can produce obvious sensitization for the fluorescence emission of Eu(Ⅲ) ion,and both the binary and ternary complexes emit stronger characteristic fluorescence of Eu(Ⅲ) ion.
Chloromethylated Polystyrene (CMPS) was first prepared with 1,4-bis (chloromethoxy) butane (BCMB) as the chloromethylation reagent. Then nucleophilic substitution between CMPS and phydroxybenzaldehyde(HBA) was conducted,resulting in benzaldehyde(BA) modified polystyrene(PS-BA) on its side chain. Finally,a reaction between 3-aminopyridine(AP) and the aldehyde group of PS-BA was allowed to form Schiff base functionalized polystyrene PS-SB. The chemical structure of PS-SB was characterized by FTIR and 1H NMR spectra. PS-SB as the first ligand and phenanthroline (Phen) as the second ligand,binary and ternary polymer-rare earth complexes,PS-(SB)3-Eu(Ⅲ) and PS-(SB)3-Eu(Ⅲ)-(Phen),were prepared,respectively. The florescence emission properties of the two complexes were preliminarily explored. The experimental results show that the rate of the nucleophilic substitution reaction between CMPS and HBA has a mechanism of SN 1. For the nucleophilic substitution reaction,N,Ndimethylacetamide(DMAC) with stronger polarity is a suitable solvent,and the temperature of 80℃ is appropriate. The macromolecular ligand PS-SB can produce obvious sensitization for the fluorescence emission of Eu(Ⅲ) ion,and both the binary and ternary complexes emit stronger characteristic fluorescence of Eu(Ⅲ) ion.
2015, 32(2): 192-199
doi: 10.11944/j.issn.1000-0518.2015.02.140185
Abstract:
O-hydroxypropyl-N-octyl chitosan(C8-HPCS) was prepared by reacting 1-octyl bromide with Ohydroxypropyl chitosan(HPCS) under microwave heating. HPCS was prepared with chitosan and propylene oxide in presence of phase transfer catalyst tetrabutylammonium bromide. The intermediate HPCS and the objective product C8-HPCS were characterized by FTIR and 1H NMR spectroscopy. The results show that C8-HPCS has an excellent integrated performance when the reaction time is 50 min,the temperature is 65℃,the dosage of bromooctane is 8 mL and the dosage of tetrabutylammonium bromide is 0.07 g. The foamability, foaming property and emulsibility are 3.9 cm,88.9% and 78.1%,respectively. The critical micelle concentration of C8-HPCS is 0.015 g/L with the surface tension of 58.5 mN/m and the hydrophile lipophile balance number is 13.44. The thermal stability analysis shows that the C8-HPCS is stable up to 270℃ and the XRD analysis indicates that the quaternized chitosan is completely amorphous.
O-hydroxypropyl-N-octyl chitosan(C8-HPCS) was prepared by reacting 1-octyl bromide with Ohydroxypropyl chitosan(HPCS) under microwave heating. HPCS was prepared with chitosan and propylene oxide in presence of phase transfer catalyst tetrabutylammonium bromide. The intermediate HPCS and the objective product C8-HPCS were characterized by FTIR and 1H NMR spectroscopy. The results show that C8-HPCS has an excellent integrated performance when the reaction time is 50 min,the temperature is 65℃,the dosage of bromooctane is 8 mL and the dosage of tetrabutylammonium bromide is 0.07 g. The foamability, foaming property and emulsibility are 3.9 cm,88.9% and 78.1%,respectively. The critical micelle concentration of C8-HPCS is 0.015 g/L with the surface tension of 58.5 mN/m and the hydrophile lipophile balance number is 13.44. The thermal stability analysis shows that the C8-HPCS is stable up to 270℃ and the XRD analysis indicates that the quaternized chitosan is completely amorphous.
2015, 32(2): 200-206
doi: 10.11944/j.issn.1000-0518.2015.02.140124
Abstract:
Auto-catalyzed film on polyester (PET) surface was prepared through chitosan (CS)/polyvinyl alcohol(PVA) complex film with PdCl2,which successfully initiated the nickel electroless plating afterwards. The CS/PVA complex film has interpenetrating networks(IPN) structure with strong hydrogen bonds in it. The chemical structure of complex film was characterized by Fourier transform infrared spectroscopic (FT-IR) analysis and tensile strength test. After electroless plating,the surface morphology, thermal stability, electromagnetic shielding effectiveness (SE) and adhesion strength of the metallized PET fabric were investigated by scanning electron microscopy(SEM),thermogravimetry(TG),SE test and washing fastness test. The results show that the nickel layer can be obtained on treated PET fabrics with good conductivity,fine uniformity and strong adhesion strength.
Auto-catalyzed film on polyester (PET) surface was prepared through chitosan (CS)/polyvinyl alcohol(PVA) complex film with PdCl2,which successfully initiated the nickel electroless plating afterwards. The CS/PVA complex film has interpenetrating networks(IPN) structure with strong hydrogen bonds in it. The chemical structure of complex film was characterized by Fourier transform infrared spectroscopic (FT-IR) analysis and tensile strength test. After electroless plating,the surface morphology, thermal stability, electromagnetic shielding effectiveness (SE) and adhesion strength of the metallized PET fabric were investigated by scanning electron microscopy(SEM),thermogravimetry(TG),SE test and washing fastness test. The results show that the nickel layer can be obtained on treated PET fabrics with good conductivity,fine uniformity and strong adhesion strength.
2015, 32(2): 207-213
doi: 10.11944/j.issn.1000-0518.2015.02.140168
Abstract:
Fluorine modified catalyst was prepared by introducing different content of fluorine during the preparation of PtSnNaLa/ZSM-5. These catalysts were used for the dehydrogenation of propane. The effect of fluorine addition on the structure,surface acidity and reaction performance of the catalysts were studied by means of XRD,NH3-TPD,FT-IR,27Al MAS NMR and TPR. The results indicate that the addition of fluorine reduced the weak-acid strength of the catalyst,but had no obvious influence on the catalyst structure. Meanwhile,the existence of fluorine strengthened the interaction between Pt and the support,and caused the dealumination of the support to some extent. As a result,the reduction of Sn component becomes relatively easy. The influence of fluoride addition on the reaction performance is mainly concentrated on improving the selectivity to propene. As for the catalyst with 0.2% fluoride,the selectivity towards propene can reach 99.2% after the reaction for 7 h.
Fluorine modified catalyst was prepared by introducing different content of fluorine during the preparation of PtSnNaLa/ZSM-5. These catalysts were used for the dehydrogenation of propane. The effect of fluorine addition on the structure,surface acidity and reaction performance of the catalysts were studied by means of XRD,NH3-TPD,FT-IR,27Al MAS NMR and TPR. The results indicate that the addition of fluorine reduced the weak-acid strength of the catalyst,but had no obvious influence on the catalyst structure. Meanwhile,the existence of fluorine strengthened the interaction between Pt and the support,and caused the dealumination of the support to some extent. As a result,the reduction of Sn component becomes relatively easy. The influence of fluoride addition on the reaction performance is mainly concentrated on improving the selectivity to propene. As for the catalyst with 0.2% fluoride,the selectivity towards propene can reach 99.2% after the reaction for 7 h.
2015, 32(2): 214-220
doi: 10.11944/j.issn.1000-0518.2015.02.140133
Abstract:
A Strandberg-type molybdophosphate {H4(H2biim)5(C(NH2)3)4}[H2P2Mo5O23]2·8H2O (1, H2 biim=2,2'-biimidazole) modified by 2,2'-biimidazole and guanidinium cations was self-assembled in aqueous solution of pH=3~4 containing sodium molybdate,2,2'-biimidazole,guanidine hydrochloride,and an excess of phosphoric acid,and was characterized by single crystal X-ray diffraction analysis,infrared spectroscopy(FT-IR),themogravimetry-differential thermal analysis(TG-DTA) and X-ray powder diffraction (XRD). Compound 1 has a stable 3D organic-inorganic hybrid framework. It was used as a catalyst for carbonyl-protection. The synthesis of cyclohexanone ethylene ketal was performed as an example to investigate some influence factors on the yield,such as catalyst loading,molar ratio of reactants and reaction time. The optimal conditions are:the molar ratio of catalyst(based on Mo) to ketone is 1:300,the molar ratio of ketone to alcohol is 1:1.4,and reaction time is 2.5 h. The catalytic activity of compound 1 for the synthesis of four other ketals was evaluated. The results show that compound 1 is a better catalyst for the synthesis of cyclohexanone ethylene ketal.
A Strandberg-type molybdophosphate {H4(H2biim)5(C(NH2)3)4}[H2P2Mo5O23]2·8H2O (1, H2 biim=2,2'-biimidazole) modified by 2,2'-biimidazole and guanidinium cations was self-assembled in aqueous solution of pH=3~4 containing sodium molybdate,2,2'-biimidazole,guanidine hydrochloride,and an excess of phosphoric acid,and was characterized by single crystal X-ray diffraction analysis,infrared spectroscopy(FT-IR),themogravimetry-differential thermal analysis(TG-DTA) and X-ray powder diffraction (XRD). Compound 1 has a stable 3D organic-inorganic hybrid framework. It was used as a catalyst for carbonyl-protection. The synthesis of cyclohexanone ethylene ketal was performed as an example to investigate some influence factors on the yield,such as catalyst loading,molar ratio of reactants and reaction time. The optimal conditions are:the molar ratio of catalyst(based on Mo) to ketone is 1:300,the molar ratio of ketone to alcohol is 1:1.4,and reaction time is 2.5 h. The catalytic activity of compound 1 for the synthesis of four other ketals was evaluated. The results show that compound 1 is a better catalyst for the synthesis of cyclohexanone ethylene ketal.
2015, 32(2): 221-224
doi: 10.11944/j.issn.1000-0518.2015.02.140177
Abstract:
Protective agent free cobalt-island film with infrared enhancement effect was prepared on aluminum metal surface by replacement reaction. Its morphology and characteristics were investigated by using SEM, XRD and IR. Cobalt deposited on aluminum surface emerged as an island structure. Cobalt island films were formed by a large number of secondary cobalt particles and a small amount of cobalt particles through a close packing pattern. Cobalt's unique structure enables a significant enhancement effect on infrared absorption spectrum of organic molecules which are adsorbed on the surface of silver particles. The infrared spectroscopy of 1 mmol/L para-mercaptobenzoic acid has been greatly enhanced on the cobalt-island film. Therefore,the surface-enhanced infrared spectroscopy can be used for trace analysis and testing.
Protective agent free cobalt-island film with infrared enhancement effect was prepared on aluminum metal surface by replacement reaction. Its morphology and characteristics were investigated by using SEM, XRD and IR. Cobalt deposited on aluminum surface emerged as an island structure. Cobalt island films were formed by a large number of secondary cobalt particles and a small amount of cobalt particles through a close packing pattern. Cobalt's unique structure enables a significant enhancement effect on infrared absorption spectrum of organic molecules which are adsorbed on the surface of silver particles. The infrared spectroscopy of 1 mmol/L para-mercaptobenzoic acid has been greatly enhanced on the cobalt-island film. Therefore,the surface-enhanced infrared spectroscopy can be used for trace analysis and testing.
2015, 32(2): 225-231
doi: 10.11944/j.issn.1000-0518.2015.02.140139
Abstract:
A poly p-aminobenzene sulfonic acid (ABSA) modified glassy carbon electrode (GCE) was prepared by electroploymerization. The electrochemical behavior of pyridoxine hydrochloride (VB6) was studied by cyclic voltammetry(CV) and differential pulse voltammetry(DPV) on the modified electrode. The results show that the oxidation current of VB6 on the modified electrode increases remarkably 7.5 times as that on the bare GCE. The electrode reaction of VB6 on PABSA/GCE is an diffuse-limited irreversible oxidation process involving one electron and two protons in the pH 3.0~6.5 acetate buffer. Under optimized conditions,DPV was utilized for the measurement of VB6. The linear range for the quantitative determination of VB6 is 0.04~100 μmol/L and the limit of detection is 0.01 μmol/L. This is the lowest detection limit of the known reported electrochemical analytical methods for the determination of VB6. The proposed method was applied to the analysis of VB6 tablets rapidly with recoveries between 106% and 108%.
A poly p-aminobenzene sulfonic acid (ABSA) modified glassy carbon electrode (GCE) was prepared by electroploymerization. The electrochemical behavior of pyridoxine hydrochloride (VB6) was studied by cyclic voltammetry(CV) and differential pulse voltammetry(DPV) on the modified electrode. The results show that the oxidation current of VB6 on the modified electrode increases remarkably 7.5 times as that on the bare GCE. The electrode reaction of VB6 on PABSA/GCE is an diffuse-limited irreversible oxidation process involving one electron and two protons in the pH 3.0~6.5 acetate buffer. Under optimized conditions,DPV was utilized for the measurement of VB6. The linear range for the quantitative determination of VB6 is 0.04~100 μmol/L and the limit of detection is 0.01 μmol/L. This is the lowest detection limit of the known reported electrochemical analytical methods for the determination of VB6. The proposed method was applied to the analysis of VB6 tablets rapidly with recoveries between 106% and 108%.
2015, 32(2): 232-238
doi: 10.11944/j.issn.1000-0518.2015.02.140161
Abstract:
By Alder method zinc tetraphenylporphyrin complex was synthesized and its structure was characterized. Zinc tetraphenylporphyrin film was deposited onto the surface of single mode potassium ion (K+) exchanged glass optical waveguide(OWG) by spin coater. The OWG sensor was fixed on the gas sensor system to detect volatile organic compound gases. This sensor has can respond towards low concentration of styrene,xylene,and toluene gases at room temperature. Among them styrene gas has the best response. The response and recovery time of styrene gas in 1×10-9 (V(Styrene)/V(Air)) volume fraction were 2 s and 7 s, respectively. The sensor has high sensitivity,fast response,recovery speed,and good reversibility.
By Alder method zinc tetraphenylporphyrin complex was synthesized and its structure was characterized. Zinc tetraphenylporphyrin film was deposited onto the surface of single mode potassium ion (K+) exchanged glass optical waveguide(OWG) by spin coater. The OWG sensor was fixed on the gas sensor system to detect volatile organic compound gases. This sensor has can respond towards low concentration of styrene,xylene,and toluene gases at room temperature. Among them styrene gas has the best response. The response and recovery time of styrene gas in 1×10-9 (V(Styrene)/V(Air)) volume fraction were 2 s and 7 s, respectively. The sensor has high sensitivity,fast response,recovery speed,and good reversibility.
2015, 32(2): 239-244
doi: 10.11944/j.issn.1000-0518.2015.02.140136
Abstract:
The chemical compositions of volatile oil and fatty acid in Tamarix chinensis fruit were studied for the first time. Pharmacopoeia extraction and Soxhlet extraction methods were selected to separate the volatile oils and fatty acids. The extracts were analyzed by GC-MS technology. The matching rate between the results and standard NIST2011 spectra is over 80%. Fourty eight kinds of volatile oils and 19 kinds of fatty acids were identified. The main components of volatile oils include aromatic compounds(43.71%),aldehydes and ketones(20.58%),fatty acids(13.03%),esters(17.36%),alcohols(4.19%),etc. The main components of fatty acids include hexadecanoic acid(35.61%),linoleic acid(27.26%),oleic acid(11.33%),etc. The unsaturated fatty acid content is 38.65% in the total fatty acids. Tamarix chinensis fruit containing rich volatile oils and unsaturated fatty acids is preferable for potential utilization.
The chemical compositions of volatile oil and fatty acid in Tamarix chinensis fruit were studied for the first time. Pharmacopoeia extraction and Soxhlet extraction methods were selected to separate the volatile oils and fatty acids. The extracts were analyzed by GC-MS technology. The matching rate between the results and standard NIST2011 spectra is over 80%. Fourty eight kinds of volatile oils and 19 kinds of fatty acids were identified. The main components of volatile oils include aromatic compounds(43.71%),aldehydes and ketones(20.58%),fatty acids(13.03%),esters(17.36%),alcohols(4.19%),etc. The main components of fatty acids include hexadecanoic acid(35.61%),linoleic acid(27.26%),oleic acid(11.33%),etc. The unsaturated fatty acid content is 38.65% in the total fatty acids. Tamarix chinensis fruit containing rich volatile oils and unsaturated fatty acids is preferable for potential utilization.
