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2019 Volume 36 Issue 7
2019, 36(7): 733-748
doi: 10.11944/j.issn.1000-0518.2019.07.190040
Abstract:
In recent years, with the rising incidence of cancer, the renewal and development of cancer therapy technology is particularly important. Especially, the introduction of chemotherapy has promoted the research for the release system of fluorescence small molecule anticancer drugs. An anticancer drug release system combines organic fluorescent molecules with anticancer drugs based on fluorescent effect, which has the characteristics of low toxicity, excellent targeting to cancer cells and convenience to track and monitor. Therefore, design of prodrugs with different properties can be used to study the kinetic process of the release of anticancer drugs and provide a powerful tool for the accurate treatment for cancers. This paper mainly introduces the research progress of prodrugs based on camptothecin, SN-38 and adriamycin, and the prospects for their development.
In recent years, with the rising incidence of cancer, the renewal and development of cancer therapy technology is particularly important. Especially, the introduction of chemotherapy has promoted the research for the release system of fluorescence small molecule anticancer drugs. An anticancer drug release system combines organic fluorescent molecules with anticancer drugs based on fluorescent effect, which has the characteristics of low toxicity, excellent targeting to cancer cells and convenience to track and monitor. Therefore, design of prodrugs with different properties can be used to study the kinetic process of the release of anticancer drugs and provide a powerful tool for the accurate treatment for cancers. This paper mainly introduces the research progress of prodrugs based on camptothecin, SN-38 and adriamycin, and the prospects for their development.
2019, 36(7): 749-757
doi: 10.11944/j.issn.1000-0518.2019.07.180381
Abstract:
Protein tyrosine phosphatase-1B(PTP1B) is an important target for anti-diabetic treatment. That means the creation of PTP1B inhibitors with excellent activity is undoubtedly of great significance. In this paper, eleven molecules with novel structures(ZLXZ1-ZLXZ11) containing 1, 3-selenazole and 1, 2, 4-triazole active blocks were designed and synthesized. Their structures were characterized by Fourier transform infrared spectrometer(FTIR), nuclear magnetic resonance spectroscopy(NMR) and high resolution mass spectrometry(HRMS). First, ZLXZ1 and ZLXZ11 were selected for molecular docking simulation with PTP1B on MOE 2015.10. As a result, π-H action and hydrogen bonding are formed respectively between the selenium atom on the selenazole ring in ZLXZ1 and the secondary catalytic sites Tyr46 and Asp48 in PTP1B. The selenium atom on the selenazole in the ZLXZ11 molecule forms a hydrogen bond with Asp 181, which facilitates the binding of the molecule to PTP1B. On this basis, the inhibitory activities of 11 target molecules were evaluated. The results show that the inhibition rates of the target molecules are all above 87.02%, in which three target molecules are better than that of the positive control, oleanolic acid, which indicates that these novel structures are expected to be potential PTP1B inhibitors.
Protein tyrosine phosphatase-1B(PTP1B) is an important target for anti-diabetic treatment. That means the creation of PTP1B inhibitors with excellent activity is undoubtedly of great significance. In this paper, eleven molecules with novel structures(ZLXZ1-ZLXZ11) containing 1, 3-selenazole and 1, 2, 4-triazole active blocks were designed and synthesized. Their structures were characterized by Fourier transform infrared spectrometer(FTIR), nuclear magnetic resonance spectroscopy(NMR) and high resolution mass spectrometry(HRMS). First, ZLXZ1 and ZLXZ11 were selected for molecular docking simulation with PTP1B on MOE 2015.10. As a result, π-H action and hydrogen bonding are formed respectively between the selenium atom on the selenazole ring in ZLXZ1 and the secondary catalytic sites Tyr46 and Asp48 in PTP1B. The selenium atom on the selenazole in the ZLXZ11 molecule forms a hydrogen bond with Asp 181, which facilitates the binding of the molecule to PTP1B. On this basis, the inhibitory activities of 11 target molecules were evaluated. The results show that the inhibition rates of the target molecules are all above 87.02%, in which three target molecules are better than that of the positive control, oleanolic acid, which indicates that these novel structures are expected to be potential PTP1B inhibitors.
2019, 36(7): 758-763
doi: 10.11944/j.issn.1000-0518.2019.07.180340
Abstract:
Cinchona alkaloid derivatives as organocatalysts were applied in asymmetric Mannich reaction of isocyanoacetate with N-tosyl aryl aldimines. The effect of solvent, temperature and catalyst loading ammount were investigated. The optimized conditions were confirmed to include toluene as the solvent with a molar fraction 10% loading of catalyst 1b at room temperature. The desired products were obtained in 55%~80% yield with high diastereo- and enantioselectivities(trans/cis up to >99:1 and 82%ee).
Cinchona alkaloid derivatives as organocatalysts were applied in asymmetric Mannich reaction of isocyanoacetate with N-tosyl aryl aldimines. The effect of solvent, temperature and catalyst loading ammount were investigated. The optimized conditions were confirmed to include toluene as the solvent with a molar fraction 10% loading of catalyst 1b at room temperature. The desired products were obtained in 55%~80% yield with high diastereo- and enantioselectivities(trans/cis up to >99:1 and 82%ee).
2019, 36(7): 764-772
doi: 10.11944/j.issn.1000-0518.2019.07.180365
Abstract:
Organophosphorus compounds bearing C-S-P(O) bonds have received increasing attention due to their well-documented biological properties in the fields of pharmaceuticals and agrochemicals. We have developed a novel, simple and efficient carbon (alkyl)-sulfur-phosphorus bond-forming reaction to access S-alkyl phosphorothioates. This transformation would provide a new pathway for the formation of P-S and C-S bonds in one reaction. Altogether, seventeen S-benzyl phosphothioates were prepared in 70%~99% yields by a one-pot CsCO3-promoted coupling reaction of benzyl chloride, elemental sulfur, and H-phosphonates. Among them, thirteen pharmacologically and synthetically important S-alkyl phosphorothioates were synthesized in 45%~93% yields under air in the presence of triethylamine without any transition metal catalysts. In addition, utilization of common and readily available sulfur powder (S8) and R2P(O)H compounds as the components should make this multicomponent reaction much more attractive both fundamentally and synthetically.
Organophosphorus compounds bearing C-S-P(O) bonds have received increasing attention due to their well-documented biological properties in the fields of pharmaceuticals and agrochemicals. We have developed a novel, simple and efficient carbon (alkyl)-sulfur-phosphorus bond-forming reaction to access S-alkyl phosphorothioates. This transformation would provide a new pathway for the formation of P-S and C-S bonds in one reaction. Altogether, seventeen S-benzyl phosphothioates were prepared in 70%~99% yields by a one-pot CsCO3-promoted coupling reaction of benzyl chloride, elemental sulfur, and H-phosphonates. Among them, thirteen pharmacologically and synthetically important S-alkyl phosphorothioates were synthesized in 45%~93% yields under air in the presence of triethylamine without any transition metal catalysts. In addition, utilization of common and readily available sulfur powder (S8) and R2P(O)H compounds as the components should make this multicomponent reaction much more attractive both fundamentally and synthetically.
2019, 36(7): 773-781
doi: 10.11944/j.issn.1000-0518.2019.07.180401
Abstract:
A new hyperbranched bispyridineimine ligand was derived from 1.0 generation hyperbranched macromolecules and 2-chloro-4-methylpyridine through substitution reaction. Multinuclear chromium complex was synthesized from the reaction with chromium(Ⅲ) chloride tetrahydrofuran complex. The structure of hyperbranched bispyridineimine ligand and chromium complex were characterized by ultraviolet-visible spectrophotometer(UV-Vis), Fourier transform infrared spectroscopy(FT-IR), proton nuclear magnetic resonance(1H NMR), and electrospray ionization mass spectrometer(ESI-MS) and elemental analysis. The result accords with what we designed theoretically. The novel hyperbranched chromium complex was evaluated as catalyst precursor in the ethylene oligomerization, using methylaluminoxane(MAO) as an activator. At the same time, we investigated the effects of reaction temperature, ethylene pressure, Al/Cr molar ratio, co-catalysts and solvents on the catalytic activity and product selectivity. The oligomerization results show that the activity of the catalyst is 1.32×105 g/(mol(Cr)·h) and the selectivity for C6 and C8 reaches up to 59.30% at 45℃ and 4 MPa, Al/Cr molar ratio of 300 and 7 μmol catalyst loading with MAO as co-catalyst in toluene.
A new hyperbranched bispyridineimine ligand was derived from 1.0 generation hyperbranched macromolecules and 2-chloro-4-methylpyridine through substitution reaction. Multinuclear chromium complex was synthesized from the reaction with chromium(Ⅲ) chloride tetrahydrofuran complex. The structure of hyperbranched bispyridineimine ligand and chromium complex were characterized by ultraviolet-visible spectrophotometer(UV-Vis), Fourier transform infrared spectroscopy(FT-IR), proton nuclear magnetic resonance(1H NMR), and electrospray ionization mass spectrometer(ESI-MS) and elemental analysis. The result accords with what we designed theoretically. The novel hyperbranched chromium complex was evaluated as catalyst precursor in the ethylene oligomerization, using methylaluminoxane(MAO) as an activator. At the same time, we investigated the effects of reaction temperature, ethylene pressure, Al/Cr molar ratio, co-catalysts and solvents on the catalytic activity and product selectivity. The oligomerization results show that the activity of the catalyst is 1.32×105 g/(mol(Cr)·h) and the selectivity for C6 and C8 reaches up to 59.30% at 45℃ and 4 MPa, Al/Cr molar ratio of 300 and 7 μmol catalyst loading with MAO as co-catalyst in toluene.
2019, 36(7): 782-789
doi: 10.11944/j.issn.1000-0518.2019.07.180346
Abstract:
Ni-P co-doped hyper-cross-linked polymer(HCP-(BTP-Ni)) was constructed in situ via cross-linking with bis(triphenylphosphine)nickel chloride(BTP-Ni). The specific surface area of HCP-(BTP-Ni) was controlled in the synthesis. The characterization results of nitrogen absorption and desorption(BET), scanning electron microscope(SEM), X-ray photoelectron spectroscopy(XPS), and others showed that the specific surface areas of HCP-(BTP-Ni) could reach 733.8 m2/g, and the conversion rate of 4-nitrophenol at room temperature could reach 99% within 8 min. The turnover frequency(TOF) could reach more than 820 h-1. At the same time, Ni-P co-doped skeleton structure greatly promoted the stability of the catalyst. The catalyst HCP-(BTP-Ni) could be reused for 8 times with a high yield.>
Ni-P co-doped hyper-cross-linked polymer(HCP-(BTP-Ni)) was constructed in situ via cross-linking with bis(triphenylphosphine)nickel chloride(BTP-Ni). The specific surface area of HCP-(BTP-Ni) was controlled in the synthesis. The characterization results of nitrogen absorption and desorption(BET), scanning electron microscope(SEM), X-ray photoelectron spectroscopy(XPS), and others showed that the specific surface areas of HCP-(BTP-Ni) could reach 733.8 m2/g, and the conversion rate of 4-nitrophenol at room temperature could reach 99% within 8 min. The turnover frequency(TOF) could reach more than 820 h-1. At the same time, Ni-P co-doped skeleton structure greatly promoted the stability of the catalyst. The catalyst HCP-(BTP-Ni) could be reused for 8 times with a high yield.>
2019, 36(7): 790-797
doi: 10.11944/j.issn.1000-0518.2019.07.180326
Abstract:
Heavy calcium powder is widely used as a filler in rubber processing, but the interface with the rubber material is poorly combined due to high polarity and poor dispersibility of powders, which affects the mechanical properties such as tensile strength and elongation at break of the rubber product. In this paper, the precipitation method is used to form calcium carbonate which is directly crystallized on the surface of heavy calcium powder particles in CaCl2-H2O-NH3-CO2 system. If n(CaCl2):n(heavy calcium powder)=1:100, 5:100, 10:100 coated calcium powder are filled into natural rubber and recycled rubber, the mechanical properties of rubber are some what improved compared to rubber filled with uncoated calcium powder. The filling amount is 8.5% and 15%, in the mechanical properties such as hardness and modulus, the coated calcium powder rubber product is obviously superior to the light calcium powder rubber product; when it comes to 5% or 8.5%, the tensile strength and elongation at break of the coated heavy calcium rubber product are close to that of silica, and the hardness is higher than rubber products filled with silica.
Heavy calcium powder is widely used as a filler in rubber processing, but the interface with the rubber material is poorly combined due to high polarity and poor dispersibility of powders, which affects the mechanical properties such as tensile strength and elongation at break of the rubber product. In this paper, the precipitation method is used to form calcium carbonate which is directly crystallized on the surface of heavy calcium powder particles in CaCl2-H2O-NH3-CO2 system. If n(CaCl2):n(heavy calcium powder)=1:100, 5:100, 10:100 coated calcium powder are filled into natural rubber and recycled rubber, the mechanical properties of rubber are some what improved compared to rubber filled with uncoated calcium powder. The filling amount is 8.5% and 15%, in the mechanical properties such as hardness and modulus, the coated calcium powder rubber product is obviously superior to the light calcium powder rubber product; when it comes to 5% or 8.5%, the tensile strength and elongation at break of the coated heavy calcium rubber product are close to that of silica, and the hardness is higher than rubber products filled with silica.
2019, 36(7): 798-806
doi: 10.11944/j.issn.1000-0518.2019.07.180389
Abstract:
At present, there are many preparation methods for superhydrophobic materials, but most of them have the disadvantages of complicated preparation processes. In this paper, the traditional free radical polymerization method was used to prepare super-hydrophobic materials with excellent performance by simple operation using organic and inorganic materials commonly used in the market as raw materials. The method for preparing superhydrophobic materials in this study can be widely applied to hydrophobic modification of various substrate materials. The crosslinkable precursor polymer P(GMA-r-St) was synthesized by conventional radical polymerization using glycidyl methacrylate(GMA) and styrene(St) as monomers. Further, it was graft-modified with trifluoroacetic acid(TFA) to prepare a fluorine-containing epoxy polymer P(GMA-r-St)-g-TFA. Nano-silica(SiO2) was modified by γ-aminopropyltriethoxysilane(KH-550) and characterized by Fourier transform infrared spectroscopy(FTIR) and thermogravimetry(TG). A superhydrophobic modified material prepared by mixing amino-modified nano-silica with a fluorine-containing epoxy polymer, and the surface of the cotton fabric is soaked to rapidly construct a super-hydrophobic structure. By changing the content of modified nanoparticles, the hydrophobic properties and solvent resistance of the constructed cotton fabrics were investigated. The results show that the cotton fabric with immersion modification has a water contact angle of 160° and a solvent resistance time of 130 min, which has good solvent resistance.
At present, there are many preparation methods for superhydrophobic materials, but most of them have the disadvantages of complicated preparation processes. In this paper, the traditional free radical polymerization method was used to prepare super-hydrophobic materials with excellent performance by simple operation using organic and inorganic materials commonly used in the market as raw materials. The method for preparing superhydrophobic materials in this study can be widely applied to hydrophobic modification of various substrate materials. The crosslinkable precursor polymer P(GMA-r-St) was synthesized by conventional radical polymerization using glycidyl methacrylate(GMA) and styrene(St) as monomers. Further, it was graft-modified with trifluoroacetic acid(TFA) to prepare a fluorine-containing epoxy polymer P(GMA-r-St)-g-TFA. Nano-silica(SiO2) was modified by γ-aminopropyltriethoxysilane(KH-550) and characterized by Fourier transform infrared spectroscopy(FTIR) and thermogravimetry(TG). A superhydrophobic modified material prepared by mixing amino-modified nano-silica with a fluorine-containing epoxy polymer, and the surface of the cotton fabric is soaked to rapidly construct a super-hydrophobic structure. By changing the content of modified nanoparticles, the hydrophobic properties and solvent resistance of the constructed cotton fabrics were investigated. The results show that the cotton fabric with immersion modification has a water contact angle of 160° and a solvent resistance time of 130 min, which has good solvent resistance.
2019, 36(7): 807-814
doi: 10.11944/j.issn.1000-0518.2019.07.180411
Abstract:
The effects of particle size and distribution of six commercial polyacrylic superabsorbent resins(SAP) on the critical concentration of gel formation were studied. The compositions of the samples were analyzed by infrared spectroscopy and X-ray photoelectron spectroscopy. The size and distribution of particles of dry samples were counted by using polarized light microscopy and ImageJ software, and were estimated by measuring the expansion ratio of the sample after water absorption. The critical gelation concentration of these superabsorbent resins was determined by rheological method and inverted experiment. The results show that the effect of the particle sizes of the six commercial polyacrylic superabsorbent resins on gel formation is not consistent with the corresponding theoretical prediction, which is caused by the uneven width of the particle size distribution. In the uniform range dominated by particle size distribution, the critical gelation concentration of the sample decreases with the increase of particle size.
The effects of particle size and distribution of six commercial polyacrylic superabsorbent resins(SAP) on the critical concentration of gel formation were studied. The compositions of the samples were analyzed by infrared spectroscopy and X-ray photoelectron spectroscopy. The size and distribution of particles of dry samples were counted by using polarized light microscopy and ImageJ software, and were estimated by measuring the expansion ratio of the sample after water absorption. The critical gelation concentration of these superabsorbent resins was determined by rheological method and inverted experiment. The results show that the effect of the particle sizes of the six commercial polyacrylic superabsorbent resins on gel formation is not consistent with the corresponding theoretical prediction, which is caused by the uneven width of the particle size distribution. In the uniform range dominated by particle size distribution, the critical gelation concentration of the sample decreases with the increase of particle size.
2019, 36(7): 815-822
doi: 10.11944/j.issn.1000-0518.2019.07.180410
Abstract:
Gel electrolyte based on pure polyvinylidene fluoride-six fluoropropene copolymer(PVDF-HFP) often suffers from low ionic conductivity, which hinders its application in dye-sensitized solar cells(DSSCs). However, the ionic conductivity of gel electrolyte and the conversion efficiency of the DSSCs can be enhanced by nanofillers. In this paper, we employed functionalized multi-walled carbon nanotube(f-MWCNT) as the nanofiller in the gel electrolyte based on PVDF-HFP. We studied its effect on ionic conductivity and ionic diffusion of electrolytes via changing the mass fraction of f-MWCNT, and investigated its improvement on the conversion efficiency and long-term stability of DSSCs. It was found that the PVDF-HFP gel electrolyte with 0.5% f-MWCNT significantly increased the ionic conductivity and ionic diffusion coefficient of the electrolyte. Moreover, the optimal conversion efficiency of the DSSCs with gel electrolyte reaches to 5.28%, which is 31.7% higher than that of the DSSCs with unfilled gel electrolyte(4.01%). After 42 days, the DSSCs still maintained 86.5% of the original conversion efficiency. The experiment confirms the great potential of f-MWCNT as the nanofiller, providing a reference for the study to improve the performance of the gel electrolyte DSSCs by nanofillers.
Gel electrolyte based on pure polyvinylidene fluoride-six fluoropropene copolymer(PVDF-HFP) often suffers from low ionic conductivity, which hinders its application in dye-sensitized solar cells(DSSCs). However, the ionic conductivity of gel electrolyte and the conversion efficiency of the DSSCs can be enhanced by nanofillers. In this paper, we employed functionalized multi-walled carbon nanotube(f-MWCNT) as the nanofiller in the gel electrolyte based on PVDF-HFP. We studied its effect on ionic conductivity and ionic diffusion of electrolytes via changing the mass fraction of f-MWCNT, and investigated its improvement on the conversion efficiency and long-term stability of DSSCs. It was found that the PVDF-HFP gel electrolyte with 0.5% f-MWCNT significantly increased the ionic conductivity and ionic diffusion coefficient of the electrolyte. Moreover, the optimal conversion efficiency of the DSSCs with gel electrolyte reaches to 5.28%, which is 31.7% higher than that of the DSSCs with unfilled gel electrolyte(4.01%). After 42 days, the DSSCs still maintained 86.5% of the original conversion efficiency. The experiment confirms the great potential of f-MWCNT as the nanofiller, providing a reference for the study to improve the performance of the gel electrolyte DSSCs by nanofillers.
2019, 36(7): 823-831
doi: 10.11944/j.issn.1000-0518.2019.07.190021
Abstract:
A simple and efficient capillary electrochromatography-electrospray- time of flight/mass spectrometry(CEC-ESI-TOF/MS) method for the separation and analysis of mixed amino acid enantiomers was established. D, L-arginine, D, L-valine, and D, L-glutamate acid were taken as the research objects. By optimizing the CEC separation conditions and MS detection conditions, the six components of the three mixed amino acid enantiomers were separated within 15 min, and the resolutions were 3.03, 1.59 and 1.37, respectively. It provides a reference method for the separation and analysis of mixed enantiomers.
A simple and efficient capillary electrochromatography-electrospray- time of flight/mass spectrometry(CEC-ESI-TOF/MS) method for the separation and analysis of mixed amino acid enantiomers was established. D, L-arginine, D, L-valine, and D, L-glutamate acid were taken as the research objects. By optimizing the CEC separation conditions and MS detection conditions, the six components of the three mixed amino acid enantiomers were separated within 15 min, and the resolutions were 3.03, 1.59 and 1.37, respectively. It provides a reference method for the separation and analysis of mixed enantiomers.
2019, 36(7): 832-838
doi: 10.11944/j.issn.1000-0518.2019.07.180391
Abstract:
The pretreatment procedure of enzymatic hydrolysis and extraction coupled with solid phase extraction(SPE) purification is usually employed for the determination of β-agonists by high performance liquid chromatography(HPLC) with tandam mass spetroscopy(MS) in food originated from animals. In this study, a HPLC-MS/MS with QuEChERS(Quick, Easy, Cheap, Effective, Rugged, Safe) purification procedures was developed for the determination of terbutaline, salbutamol, ractopamine and clenbuterol in food of animal origin using both acid hydrolysis extraction method and enzymatic hydrolysis extraction method in food poisoning event caused by clenbuterol and analogs. Using enzymatic hydrolysis extraction with QuEChERS purification and electrospray ionization mass spectrometry in positive mode adopting multiple reaction monitoring(MRM) mode, four analytes were analyzed in the range of 1.0~20.0 μg/L with correlation coefficients(R) higher than 0.999. The limit of detection(LOD) and the limit of quantification(LOQ) was 0.1 μg/kg and 0.3 μg/kg, respectively, and recoveries for 4 β2-agonists in pork and beef samples ranged from 78.5% to 112% with relative standard deviation(RSD) of 2.8%~8.9%. When acid hydrolysis extraction was used alternatively, the pretreatment time was shortened greatly, but the result for ractopamine was slightly lower than that using the enzymatic hydrolysis extraction procedure. The combined use of two pretreatment procedures will promote the emergency response in real food poisoning case caused by clenbuterol and analogs.
The pretreatment procedure of enzymatic hydrolysis and extraction coupled with solid phase extraction(SPE) purification is usually employed for the determination of β-agonists by high performance liquid chromatography(HPLC) with tandam mass spetroscopy(MS) in food originated from animals. In this study, a HPLC-MS/MS with QuEChERS(Quick, Easy, Cheap, Effective, Rugged, Safe) purification procedures was developed for the determination of terbutaline, salbutamol, ractopamine and clenbuterol in food of animal origin using both acid hydrolysis extraction method and enzymatic hydrolysis extraction method in food poisoning event caused by clenbuterol and analogs. Using enzymatic hydrolysis extraction with QuEChERS purification and electrospray ionization mass spectrometry in positive mode adopting multiple reaction monitoring(MRM) mode, four analytes were analyzed in the range of 1.0~20.0 μg/L with correlation coefficients(R) higher than 0.999. The limit of detection(LOD) and the limit of quantification(LOQ) was 0.1 μg/kg and 0.3 μg/kg, respectively, and recoveries for 4 β2-agonists in pork and beef samples ranged from 78.5% to 112% with relative standard deviation(RSD) of 2.8%~8.9%. When acid hydrolysis extraction was used alternatively, the pretreatment time was shortened greatly, but the result for ractopamine was slightly lower than that using the enzymatic hydrolysis extraction procedure. The combined use of two pretreatment procedures will promote the emergency response in real food poisoning case caused by clenbuterol and analogs.
2019, 36(7): 847-854
doi: 10.11944/j.issn.1000-0518.2019.07.190047
Abstract:
A simple colorimetric method for determination of H2O2 and glucose was established based on the peroxidase-like activity of deuterohemin-Ala His Thr Val Glu Lys(DhHP-6) to catalyze the oxidation of 4-aminoantipyrine(4-APP)-chlorophenol color reaction system in the presence of H2O2. The effects of pH, substrate concentration and DhHP-6 concentration were observed, and the reaction linearity, stability, correlation and recovery rate of the colorimetric method were detected. Under optimal reaction conditions, the activity of DhHP-6 is superior to that of peroxidase(POD) under different temperatures and times; the Michaelis constant(Km) and maximum reaction rate(vmax) of DhHP-6 catalyzing H2O2 are 0.171 mmol/L and 4.22×10-6 mol/s, respectively; the linearity range of H2O2 response is 0.39~25.0 mmol/L, the coefficient of variation(CV) and spiked recovery of the high, medium and low levels are between 1.29%~2.16% and 94.5%~101.1%, respectively; and correlation coefficient with the commercial kit is 0.9946; the concentration of glucose in 36 blood samples are 4.26~17.48 mmol/L. There is no significant difference between the two sets of data for glucose assay kit(P>0.05). Therefore, this is a simple, cheap, convenient and sensitive colorimetric determination method.
A simple colorimetric method for determination of H2O2 and glucose was established based on the peroxidase-like activity of deuterohemin-Ala His Thr Val Glu Lys(DhHP-6) to catalyze the oxidation of 4-aminoantipyrine(4-APP)-chlorophenol color reaction system in the presence of H2O2. The effects of pH, substrate concentration and DhHP-6 concentration were observed, and the reaction linearity, stability, correlation and recovery rate of the colorimetric method were detected. Under optimal reaction conditions, the activity of DhHP-6 is superior to that of peroxidase(POD) under different temperatures and times; the Michaelis constant(Km) and maximum reaction rate(vmax) of DhHP-6 catalyzing H2O2 are 0.171 mmol/L and 4.22×10-6 mol/s, respectively; the linearity range of H2O2 response is 0.39~25.0 mmol/L, the coefficient of variation(CV) and spiked recovery of the high, medium and low levels are between 1.29%~2.16% and 94.5%~101.1%, respectively; and correlation coefficient with the commercial kit is 0.9946; the concentration of glucose in 36 blood samples are 4.26~17.48 mmol/L. There is no significant difference between the two sets of data for glucose assay kit(P>0.05). Therefore, this is a simple, cheap, convenient and sensitive colorimetric determination method.
2019, 36(7): 839-846
doi: 10.11944/j.issn.1000-0518.2019.07.180378
Abstract:
The phosphinothricin acetyltransferase(PAT) gene is a kind of exogenous DNA segments indicating genetically modified plants. In this research, a sensitive method for determination of the PAT gene in transgenic maize has been developed using reduced graphene oxide and nano zirconia(nanoZrO2) composites as a platform for immobilizing DNA probes. First, the graphene oxide was direct electrochemically reduced on a glassy carbon electrode(GCE); then, a layer of nanoZrO2 was covered on the modified electrode. Last, the DNA probes were immobilized via the affinity between phosphate groups in the DNA probes and the oxygen in nanoZrO2. The hybridization of the DNA probes with the PAT gene segments was monitored by differential pulse voltammetry(DPV). The sensor was stable, reproducible and sensitive to effectively discriminate the PAT gene in transgenic maize. The detection limit was 2.0×10-15 mol/L.
The phosphinothricin acetyltransferase(PAT) gene is a kind of exogenous DNA segments indicating genetically modified plants. In this research, a sensitive method for determination of the PAT gene in transgenic maize has been developed using reduced graphene oxide and nano zirconia(nanoZrO2) composites as a platform for immobilizing DNA probes. First, the graphene oxide was direct electrochemically reduced on a glassy carbon electrode(GCE); then, a layer of nanoZrO2 was covered on the modified electrode. Last, the DNA probes were immobilized via the affinity between phosphate groups in the DNA probes and the oxygen in nanoZrO2. The hybridization of the DNA probes with the PAT gene segments was monitored by differential pulse voltammetry(DPV). The sensor was stable, reproducible and sensitive to effectively discriminate the PAT gene in transgenic maize. The detection limit was 2.0×10-15 mol/L.
