M, a particular industrial waste, was selected to detoxify chromium slag at a high temperature. The carbon remaining in M reduced Cr ( Ⅳ ) of Na2 CrO4 borne in the chromium slag to Cr ( Ⅲ ) in the solid phase re...M, a particular industrial waste, was selected to detoxify chromium slag at a high temperature. The carbon remaining in M reduced Cr ( Ⅳ ) of Na2 CrO4 borne in the chromium slag to Cr ( Ⅲ ) in the solid phase reaction, and its thermodynamics and kinetics were studied. The reduction process of Na2CrO4 by carbon produced CO, whiCh'was endothermic. Under the experimental condition, the apparent activation energy was 4. 41 kJ·mol^-1 , the'apparent order of reaction for Na2 CrO4 was equal to one, and the partial pressure of CO was only 0.22 Pa at 1 330℃.展开更多
A sensitive flow injection chemiluminescence method has been developed for the detection of resveratrol in red wine based on the fact that resveratrol can greatly enhance chemiluminescence reaction between KMnO4 and H...A sensitive flow injection chemiluminescence method has been developed for the detection of resveratrol in red wine based on the fact that resveratrol can greatly enhance chemiluminescence reaction between KMnO4 and HCHO in sulfuric acid medium. Analytes were pre-concentrated on solid sorbents (C18 solid-phase extraction cartridges). Under the optimum conditions, the proposed method allows the measurement of resveratrol over the range of 1.32 × 10^-8 to 1.32 × 10^-5 mol/L with a detection limit of 3.30 ×10^-9 mol/L, and the relative standard deviation for 1.32 ×10^-5 mol/L resveratrol (n = 11) is 3.8%. This method has been successfully applied for the determination of the resveratrol in red wine. Furthermore, the possible reaction mechanism was also discussed.展开更多
Solid phase extraction is widely used in sample pretreatment,concentration and analysis processes due to high selectivity and suitability for low concentration sample system.In this review,we systematically summarized...Solid phase extraction is widely used in sample pretreatment,concentration and analysis processes due to high selectivity and suitability for low concentration sample system.In this review,we systematically summarized and discussed the development trends of solid phase extraction by bibliometrics method.By analyzing papers output scale,the research and development direction of solid phase extraction technology is prospected.We also give an overview on current strategies of novel solid phase extraction from the separation medium and separation technology.The paper aims to describe the global research profile and the development trends of solid phase extraction,to help researchers to accurately grasp the research trend and to provide support for scientific research institutions to formulate scientific policies and strategic plans.Furthermore,the prospect of the development and application of solid phase extraction is also discussed.展开更多
Urinary 8-hydroxy-2 -deoxyguanosine(8-OHdG) is an excellent marker of oxidative DNA damage.In this study,employing guanosine as dummy template a novel molecularly imprinted(MIP) monolithic capillary column had been sy...Urinary 8-hydroxy-2 -deoxyguanosine(8-OHdG) is an excellent marker of oxidative DNA damage.In this study,employing guanosine as dummy template a novel molecularly imprinted(MIP) monolithic capillary column had been synthesized,and that was used as medium of in-tube solid phase microextraction(SPME).Coupled with capillary electrophoresis-electrochemical detection(CE-ECD),the system of extraction and detection of 8-OHdG in urinary sample had been developed.Because of its greater phase ratio combined with conv...展开更多
The determination of the methamidaphos pesticide residue on vegetables with a simple solid phase extract(SPE) flow injection(FI) -chemiluminescence(CL) method is described. The method is based on the enhancing e...The determination of the methamidaphos pesticide residue on vegetables with a simple solid phase extract(SPE) flow injection(FI) -chemiluminescence(CL) method is described. The method is based on the enhancing effect of methamidaphos on the CL reaction of luminol with hydrogen peroxide in an alkaline solution. Under the optimal conditions, the CL intensity is linear to the methamidaphos mass concentration in a range of 0. 2-13μg/mL ( r= 0. 9992). The detection limit(3σ) is 0. 047μg/mL. The relative standard deviations for the analysis of three samples are 1.8%, 2.5% and 3.7% ( n = 5 ), respectively. The recovery is in a range of 90%-109% by the method. In this work, this method was successfully applied to the determination of the methamidaphos residue on some vegetable samples.展开更多
A fast and simple method for determination of α, β, γ-hexachlorocyclohexanes (HCHs) in water using activated carbon fiber-solid phase microextraction(ACF-SPME) were studied. Results showed the performance of adsorp...A fast and simple method for determination of α, β, γ-hexachlorocyclohexanes (HCHs) in water using activated carbon fiber-solid phase microextraction(ACF-SPME) were studied. Results showed the performance of adsorption and desorption of three HCHs on ACF were excellent. A wide linear range from 10 to 100 μg/L and detection limits of the ng/L level were obtained using ACF-SPME with GC-MS in selected ion monitoring(SIM) acquisition mode. The proposed method was also successfully applied for determination of three HCHs in tap water. Compared to commercial fibers, ACF showed some advantages such as better resistance to solvents, higher thermal stability, longer lifetime and lower cost. The data demonstrated that GC-MS with ACF-SPME is well suitable for the analysis of HCHs in water.展开更多
Velocities of solid phase and liquid phase in debris flow are one key problem to research on impact and abrasion mechanism of banks and control structures under action of debris flow. Debris flow was simplified as two...Velocities of solid phase and liquid phase in debris flow are one key problem to research on impact and abrasion mechanism of banks and control structures under action of debris flow. Debris flow was simplified as two-phase liquid composed of solid phase with the same diameter particles and liquid phase with the same mechanical features. Assume debris flow was one-dimension two-phase liquid moving to one direction, then general equations of velocities of solid phase and liquid phase were founded in two-phase theory. Methods to calculate average pressures, volume forces and surface forces of debris flow control volume were established. Specially, surface forces were ascertained using Bingham's rheology equation of liquid phase and Bagnold's testing results about interaction between particles of solid phase. Proportional coefficient of velocities between liquid phase and solid phase was put forward, meanwhile, divergent coefficient between theoretical velocity and real velocity of solid phase was provided too. To state succinctly before, method to calculate velocities of solid phase and liquid phase was obtained through solution to general equations. The method is suitable for both viscous debris flow and thin debris flow. Additionally, velocities every phase can be identified through analyzing deposits in-situ after occurring of debris flow. It is obvious from engineering case the result in the method is consistent to that in real-time field observation.展开更多
Manganese silicide MnSi_(2-x) thin films have been prepared on n-type siliconsubstrates through solid phase reaction. The heterostructures were analyzed by X-ray diffraction,Rutherford backscattering spectroscopy, Fou...Manganese silicide MnSi_(2-x) thin films have been prepared on n-type siliconsubstrates through solid phase reaction. The heterostructures were analyzed by X-ray diffraction,Rutherford backscattering spectroscopy, Fourier transform infrared transmittance spectroscopy andthe four-point probe technique. The results show that two manganese silicides have been formedsequentially via the reaction of thin layer Mn with Si substrate at different irradiation annealingstages, i.e., MnSi at 450 deg C and MnSi_(1.73) at 550 deg C. MnSi_(1.73) phase exhibits preferredgrowth after irradiation with infrared. In situ four-point probe measurements of sheet resistanceduring infrared irradiation annealing show that nucleation of MnSi and phase transformation of MnSito MaSi_(1.73) occur at 410 deg C and 530 deg C, respectively; the MnSi phase shows metallicbehavior, while MnSi_(1.73) exhibits semiconducting behavior. Characteristic phonon bands ofMnSi_(2-x) silicides, which can be used for phase identification along with conventional XRDtechniques, have been observed by FTIR spectroscopy.展开更多
Development of a novel in vivo lung perfusion(IVLP)procedure allows localized delivery of high-dose doxorubicin(DOX)for targeting residual micrometastatic disease in the lungs.However,DOX delivery via IVLP requires ca...Development of a novel in vivo lung perfusion(IVLP)procedure allows localized delivery of high-dose doxorubicin(DOX)for targeting residual micrometastatic disease in the lungs.However,DOX delivery via IVLP requires careful monitoring of drug level to ensure tissue concentrations of this agent remain in the therapeutic window.A small dimension nitinol wire coated with a sorbent of biocompatible morphology(Bio-SPME)has been clinically evaluated for in vivo lung tissue extraction and determination of DOX and its key metabolites.The in vivo Bio-SPME-IVLP experiments were performed on pig model over various(150 and 225 mg/m^(2))drug doses,and during human clinical trial.Two patients with metastatic osteosarcoma were treated with a single 5 and 7 μg/mL(respectively)dose of DOX during a 3-h IVLP.In both pig and human cases,DOX tissue levels presented similar trends during IVLP.Human lung tissue concentrations of drug ranged between 15 and 293 μg/g over the course of the IVLP procedure.In addition to DOX levels,Bio-SPME followed by liquid chromatography-mass spectrometry analysis generated 64 metabolic features during endogenous metabolite screening,providing information about lung status during drug administration.Real-time monitoring of DOX levels in the lungs can be performed effectively throughout the IVLP procedure by in vivo Bio-SPME chemical biopsy approach.Bio-SPME also extracted various endogenous molecules,thus providing a real-time snapshot of the physiology of the cells,which might assist in the tailoring of personalized treatment strategy.展开更多
The aim of this work was to develop an automated on-line solid phase extraction(SPE)with liquid chromatography-tandem mass spectrometry method for the detection of fifteen sulfonamides in pork and fish samples.Samples...The aim of this work was to develop an automated on-line solid phase extraction(SPE)with liquid chromatography-tandem mass spectrometry method for the detection of fifteen sulfonamides in pork and fish samples.Samples were extracted with 0.2%formic acid acetonitrile solution,purified by on-line SPE device with HLB column,then separated by XBridge C18 column,using 0.1%formic acid solution and acetonitrile as the mobile phase.Mass spectrometric data was acquired under multiple reaction monitoring(MRM)mode using positive ionization electrospray.Internal standard method was used in the quantification,good linear relationship was got in range of 0.1–100 ng/mL and correlation coefficient was higher than 0.9990.The limits of detection were in the range of 0.125–2.00g/kg and the limits of quantitation were in the range of 0.250–5.00g/kg.Recoveries of the method were in range of 78.3%–99.3%,relative standard deviation were lower than 10%.The method was simple,sensitivity,and could be used for routine supervision and analysis of fifteen sulfonamides in pork and fish.展开更多
Cr(Ⅵ)-based compounds pollution have attracted global concern due to serious harm to humans and environment.Hence,it is crucial to exploit an effective technique to eliminate Cr(Ⅵ)in water.Herein,we in-situ grown Bi...Cr(Ⅵ)-based compounds pollution have attracted global concern due to serious harm to humans and environment.Hence,it is crucial to exploit an effective technique to eliminate Cr(Ⅵ)in water.Herein,we in-situ grown BiOI on graphitic carbon nitride to prepare the BiOI/g-C_(3)N_(4)(BCN)direct Z-scheme heterojunction by solid phase engineering method at room temperature.Experimental result shown the photocatalytic activity of pure BiOI were obviously enhanced by constructing Z-scheme BCN heterostructure,and BCN-3 heterostructure exhibited the optimal photocatalytic degradation of RhB with 98%yield for 2.5 h and reduction of Cr(Ⅵ)with more than 99%yield for 1.5 h at pH=2.Stability test shows BCN-3 still kept more than 98%reduction efficiency after 6 cycles.In addition,we also studied the reduction mechanism that shown the.O_(2)^(-)radicals essentially helped to reduce the Cr(Ⅵ)in aqueous solution under illumination,verified the direct Z-scheme charge transfer path by X-ray photoelectron spectroscopy(XPS)and the free radical trapping experiment.The work open a new way for rationally designing photocatalyst heterostructure to reduce Cr(Ⅵ)to Cr(Ⅲ).展开更多
To establish an analytical method for determination of four bisphenols (BPA, BPB, BPF, and BPS) and two alkylphenols (4-n-OP, 4-n-NP) in water by ultra performance liquid chromatography- tandem mass spectrometry ...To establish an analytical method for determination of four bisphenols (BPA, BPB, BPF, and BPS) and two alkylphenols (4-n-OP, 4-n-NP) in water by ultra performance liquid chromatography- tandem mass spectrometry (UPLC/MS/MS). The water samples were extracted and condensed with solid-phase extraction (SPE) using C18 cartridges and eluted by acetonitrile. Separation was carried out with Acquity BEH C8 column and detection were performed by UPLC/MS/MS. Quantification was calculated by using the internal standard BPA-d16 and 4-n-NP-d8. The linear correlation coefficients of these compounds in the range of 1.0-100.0μg/L were all over 0.999. The minimum detectable concentrations were 0.75-1.0 ng/L, and the recoveries ranged from 87.0% to 106.9%.展开更多
A single crystalline Mg2Si film was formed by solid phase reaction (SPR) of a Si(111) substrate with an Mg overlayer capped with an oxide layer(s),which was enhanced by post annealing from room temperature to 10...A single crystalline Mg2Si film was formed by solid phase reaction (SPR) of a Si(111) substrate with an Mg overlayer capped with an oxide layer(s),which was enhanced by post annealing from room temperature to 100℃ in a molecular beam epitaxy (MBE) system.The thermal stability of the Mg2Si film was then systematically investigated by post annealing in an oxygen-radical ambient at 300℃,450℃ and 650℃,respectively.The Mg2Si film stayed stable until the annealing temperature reached 450℃ then it transformed into amorphous MgOx attributed to the decomposition of Mg2Si and the oxidization of dissociated Mg.展开更多
A procedure for the preconcentration of copper was described in this paper using multi-walled carbon nanotubes (MWCNTs) oxidized by potassium permanganate as the adsorbent for the enrichment of trace copper in water s...A procedure for the preconcentration of copper was described in this paper using multi-walled carbon nanotubes (MWCNTs) oxidized by potassium permanganate as the adsorbent for the enrichment of trace copper in water samples. Important parameters, such as the sample pH, the concentration and volume of eluent, sample flow rate and volume, and interference of coexisting ions, were investigated. The obtained results indicated that proposed method possessed an excellent analytical performance. The linear range, the detection limit, and precison (RSD) were 1–100 ng/mL (R(2) = 0.9993), 0.32 ng/mL and 2.88%, respectively. The results showed that copper could be adsorbed quantitatively on the pretreated MWCNTs with potassium permanganate, and proposed method was very useful in the monitoring of copper in the environment.展开更多
Base on the previous work in laboratory, a novel polyaniline doped with polydimethylsiloxane coating was developed on a stainless steel wire for solid phase microextraction(SPME) by electroplating method. This elect...Base on the previous work in laboratory, a novel polyaniline doped with polydimethylsiloxane coating was developed on a stainless steel wire for solid phase microextraction(SPME) by electroplating method. This electroplating method not only has advantages of ease preparation and simple equipments required, but also increases the lifetime of the SPME fiber. The composite fiber(polyaniline/ polydimethylsiloxane(PANI/PDMS)) was evaluated by analyzing n-tridecane, n-tetradecane and n-pentadecane in aqueous sample. The new fiber coating showed comprehensive abilities to extract alkanes compounds. The relative standard deviations were found to be 6.8%-10.33%.展开更多
Human urotension-Ⅱ was synthesized efficiently on Wang resin under microwave irradiation using Fmoc/tBu orthogonal protection strategy. Disulphide bridge was formed on solid phase with the irradiation of microwave, t...Human urotension-Ⅱ was synthesized efficiently on Wang resin under microwave irradiation using Fmoc/tBu orthogonal protection strategy. Disulphide bridge was formed on solid phase with the irradiation of microwave, then the whole peptide was cleaved from the resin. The purity of crude peptide cyclized under microwave irradiation was higher than that under room temperature.展开更多
The comparison of solid phase extraction(SPE) for the preconcentration and isolation of polyphenols in tobacco samples was carried out by ultra-high performance liquid chromatography/tandem mass spectrometry (UPLC/...The comparison of solid phase extraction(SPE) for the preconcentration and isolation of polyphenols in tobacco samples was carried out by ultra-high performance liquid chromatography/tandem mass spectrometry (UPLC/MS/MS) and multivariate analysis.Several adsorbing materials of SPE(C18,NH2,SAX and OASIS) were investigated.It was found that the C18 and OASIS cartridges can not only speed up the purification process,but also simplify the SPE operation.A UPLC/MS/MS was used for the determination of polyphenols in tobacco samples after purification.All analytes were separated and determined in 2min.The limit of detection was 0.05 ng/mL.Cluster analysis(CA) and principal component analysis(PCA) were used for the analysis of 4 varieties(flue-cured tobacco,oriental tobacco,sun-cured tobacco and burley) in order to interpret the effect of planting and machining process on the concentration of polyphenols.The different types of tobacco samples could be easily clustered by CA.PCA on the chemical composition of tobacco resulted in two principal components(PCs) that take 84.2% of the total variance.The PCA and CA indicate that the polyphenols can be used for distinguishing tobacco types.展开更多
In order to accelerate the development of relatively inexpensive antimalarials that are effective against chloroquine-resistant strains of Plasmodium falciparum, a methodology for the solid phase synthesis of chalcone...In order to accelerate the development of relatively inexpensive antimalarials that are effective against chloroquine-resistant strains of Plasmodium falciparum, a methodology for the solid phase synthesis of chalcone (1, 3-diphenyl-2-propen-1-one) analogues in reasonably high yields has been developed.展开更多
A solid phase extraction procedure of methomyl and thiodicarb from environmental water was presented. This method utilizes a 40—60 mesh activated carbon cartridge and high performance liquid chromatography (HPLC). Th...A solid phase extraction procedure of methomyl and thiodicarb from environmental water was presented. This method utilizes a 40—60 mesh activated carbon cartridge and high performance liquid chromatography (HPLC). The 40—60 mesh activated carbon works faster and yield higher adsorption efficiency. Detection limits of methomyl and thiodicarb in environmental water are 0 1 μg/L and 0 2 μg/L, respectively. Average recoveries of fortified methomyl and thiodicarb in water are in the range of 90 7%—98 8% and 88 9%—103 6%, respectively. The relative standard deviations are lower than 7%. This method is simple, rapid, accurate and precise.展开更多
基金Item Sponsored by National Natural Science Foundation of China (50234040)
文摘M, a particular industrial waste, was selected to detoxify chromium slag at a high temperature. The carbon remaining in M reduced Cr ( Ⅳ ) of Na2 CrO4 borne in the chromium slag to Cr ( Ⅲ ) in the solid phase reaction, and its thermodynamics and kinetics were studied. The reduction process of Na2CrO4 by carbon produced CO, whiCh'was endothermic. Under the experimental condition, the apparent activation energy was 4. 41 kJ·mol^-1 , the'apparent order of reaction for Na2 CrO4 was equal to one, and the partial pressure of CO was only 0.22 Pa at 1 330℃.
文摘A sensitive flow injection chemiluminescence method has been developed for the detection of resveratrol in red wine based on the fact that resveratrol can greatly enhance chemiluminescence reaction between KMnO4 and HCHO in sulfuric acid medium. Analytes were pre-concentrated on solid sorbents (C18 solid-phase extraction cartridges). Under the optimum conditions, the proposed method allows the measurement of resveratrol over the range of 1.32 × 10^-8 to 1.32 × 10^-5 mol/L with a detection limit of 3.30 ×10^-9 mol/L, and the relative standard deviation for 1.32 ×10^-5 mol/L resveratrol (n = 11) is 3.8%. This method has been successfully applied for the determination of the resveratrol in red wine. Furthermore, the possible reaction mechanism was also discussed.
基金financial support of the Natural Science Foundation of Beijing (2194086)the National Natural Science Foundation of China (Nos. 21922814, 21676273, 21961160745, 31961133019 and 21921005)
文摘Solid phase extraction is widely used in sample pretreatment,concentration and analysis processes due to high selectivity and suitability for low concentration sample system.In this review,we systematically summarized and discussed the development trends of solid phase extraction by bibliometrics method.By analyzing papers output scale,the research and development direction of solid phase extraction technology is prospected.We also give an overview on current strategies of novel solid phase extraction from the separation medium and separation technology.The paper aims to describe the global research profile and the development trends of solid phase extraction,to help researchers to accurately grasp the research trend and to provide support for scientific research institutions to formulate scientific policies and strategic plans.Furthermore,the prospect of the development and application of solid phase extraction is also discussed.
基金the support of the National Natural Science Foundation of China(No.20575051).
文摘Urinary 8-hydroxy-2 -deoxyguanosine(8-OHdG) is an excellent marker of oxidative DNA damage.In this study,employing guanosine as dummy template a novel molecularly imprinted(MIP) monolithic capillary column had been synthesized,and that was used as medium of in-tube solid phase microextraction(SPME).Coupled with capillary electrophoresis-electrochemical detection(CE-ECD),the system of extraction and detection of 8-OHdG in urinary sample had been developed.Because of its greater phase ratio combined with conv...
文摘The determination of the methamidaphos pesticide residue on vegetables with a simple solid phase extract(SPE) flow injection(FI) -chemiluminescence(CL) method is described. The method is based on the enhancing effect of methamidaphos on the CL reaction of luminol with hydrogen peroxide in an alkaline solution. Under the optimal conditions, the CL intensity is linear to the methamidaphos mass concentration in a range of 0. 2-13μg/mL ( r= 0. 9992). The detection limit(3σ) is 0. 047μg/mL. The relative standard deviations for the analysis of three samples are 1.8%, 2.5% and 3.7% ( n = 5 ), respectively. The recovery is in a range of 90%-109% by the method. In this work, this method was successfully applied to the determination of the methamidaphos residue on some vegetable samples.
文摘A fast and simple method for determination of α, β, γ-hexachlorocyclohexanes (HCHs) in water using activated carbon fiber-solid phase microextraction(ACF-SPME) were studied. Results showed the performance of adsorption and desorption of three HCHs on ACF were excellent. A wide linear range from 10 to 100 μg/L and detection limits of the ng/L level were obtained using ACF-SPME with GC-MS in selected ion monitoring(SIM) acquisition mode. The proposed method was also successfully applied for determination of three HCHs in tap water. Compared to commercial fibers, ACF showed some advantages such as better resistance to solvents, higher thermal stability, longer lifetime and lower cost. The data demonstrated that GC-MS with ACF-SPME is well suitable for the analysis of HCHs in water.
基金Project supported by the Talent Fund of the Ministry of Communication of China(No.95050508) the Fund of Western Communication of China(No.200332822047) the Key Science Fund of the Ministry of Communication of China(No.95060233)
文摘Velocities of solid phase and liquid phase in debris flow are one key problem to research on impact and abrasion mechanism of banks and control structures under action of debris flow. Debris flow was simplified as two-phase liquid composed of solid phase with the same diameter particles and liquid phase with the same mechanical features. Assume debris flow was one-dimension two-phase liquid moving to one direction, then general equations of velocities of solid phase and liquid phase were founded in two-phase theory. Methods to calculate average pressures, volume forces and surface forces of debris flow control volume were established. Specially, surface forces were ascertained using Bingham's rheology equation of liquid phase and Bagnold's testing results about interaction between particles of solid phase. Proportional coefficient of velocities between liquid phase and solid phase was put forward, meanwhile, divergent coefficient between theoretical velocity and real velocity of solid phase was provided too. To state succinctly before, method to calculate velocities of solid phase and liquid phase was obtained through solution to general equations. The method is suitable for both viscous debris flow and thin debris flow. Additionally, velocities every phase can be identified through analyzing deposits in-situ after occurring of debris flow. It is obvious from engineering case the result in the method is consistent to that in real-time field observation.
基金This work has been supported jointly by the National Natural Science Foundation ofChina (Crant No. 69806005)the Natural Scie
文摘Manganese silicide MnSi_(2-x) thin films have been prepared on n-type siliconsubstrates through solid phase reaction. The heterostructures were analyzed by X-ray diffraction,Rutherford backscattering spectroscopy, Fourier transform infrared transmittance spectroscopy andthe four-point probe technique. The results show that two manganese silicides have been formedsequentially via the reaction of thin layer Mn with Si substrate at different irradiation annealingstages, i.e., MnSi at 450 deg C and MnSi_(1.73) at 550 deg C. MnSi_(1.73) phase exhibits preferredgrowth after irradiation with infrared. In situ four-point probe measurements of sheet resistanceduring infrared irradiation annealing show that nucleation of MnSi and phase transformation of MnSito MaSi_(1.73) occur at 410 deg C and 530 deg C, respectively; the MnSi phase shows metallicbehavior, while MnSi_(1.73) exhibits semiconducting behavior. Characteristic phonon bands ofMnSi_(2-x) silicides, which can be used for phase identification along with conventional XRDtechniques, have been observed by FTIR spectroscopy.
文摘Development of a novel in vivo lung perfusion(IVLP)procedure allows localized delivery of high-dose doxorubicin(DOX)for targeting residual micrometastatic disease in the lungs.However,DOX delivery via IVLP requires careful monitoring of drug level to ensure tissue concentrations of this agent remain in the therapeutic window.A small dimension nitinol wire coated with a sorbent of biocompatible morphology(Bio-SPME)has been clinically evaluated for in vivo lung tissue extraction and determination of DOX and its key metabolites.The in vivo Bio-SPME-IVLP experiments were performed on pig model over various(150 and 225 mg/m^(2))drug doses,and during human clinical trial.Two patients with metastatic osteosarcoma were treated with a single 5 and 7 μg/mL(respectively)dose of DOX during a 3-h IVLP.In both pig and human cases,DOX tissue levels presented similar trends during IVLP.Human lung tissue concentrations of drug ranged between 15 and 293 μg/g over the course of the IVLP procedure.In addition to DOX levels,Bio-SPME followed by liquid chromatography-mass spectrometry analysis generated 64 metabolic features during endogenous metabolite screening,providing information about lung status during drug administration.Real-time monitoring of DOX levels in the lungs can be performed effectively throughout the IVLP procedure by in vivo Bio-SPME chemical biopsy approach.Bio-SPME also extracted various endogenous molecules,thus providing a real-time snapshot of the physiology of the cells,which might assist in the tailoring of personalized treatment strategy.
基金This work was supported by“National Key Research and Development Program of China”(Project No.2018YFC1603400)Science and Technology Program of Hebei Province(Project No.19225503D).
文摘The aim of this work was to develop an automated on-line solid phase extraction(SPE)with liquid chromatography-tandem mass spectrometry method for the detection of fifteen sulfonamides in pork and fish samples.Samples were extracted with 0.2%formic acid acetonitrile solution,purified by on-line SPE device with HLB column,then separated by XBridge C18 column,using 0.1%formic acid solution and acetonitrile as the mobile phase.Mass spectrometric data was acquired under multiple reaction monitoring(MRM)mode using positive ionization electrospray.Internal standard method was used in the quantification,good linear relationship was got in range of 0.1–100 ng/mL and correlation coefficient was higher than 0.9990.The limits of detection were in the range of 0.125–2.00g/kg and the limits of quantitation were in the range of 0.250–5.00g/kg.Recoveries of the method were in range of 78.3%–99.3%,relative standard deviation were lower than 10%.The method was simple,sensitivity,and could be used for routine supervision and analysis of fifteen sulfonamides in pork and fish.
基金supported by the National Natural Science Foundation of China under Grant(No.51871078)Heilongjiang Science Foundation(No.E2018028)
文摘Cr(Ⅵ)-based compounds pollution have attracted global concern due to serious harm to humans and environment.Hence,it is crucial to exploit an effective technique to eliminate Cr(Ⅵ)in water.Herein,we in-situ grown BiOI on graphitic carbon nitride to prepare the BiOI/g-C_(3)N_(4)(BCN)direct Z-scheme heterojunction by solid phase engineering method at room temperature.Experimental result shown the photocatalytic activity of pure BiOI were obviously enhanced by constructing Z-scheme BCN heterostructure,and BCN-3 heterostructure exhibited the optimal photocatalytic degradation of RhB with 98%yield for 2.5 h and reduction of Cr(Ⅵ)with more than 99%yield for 1.5 h at pH=2.Stability test shows BCN-3 still kept more than 98%reduction efficiency after 6 cycles.In addition,we also studied the reduction mechanism that shown the.O_(2)^(-)radicals essentially helped to reduce the Cr(Ⅵ)in aqueous solution under illumination,verified the direct Z-scheme charge transfer path by X-ray photoelectron spectroscopy(XPS)and the free radical trapping experiment.The work open a new way for rationally designing photocatalyst heterostructure to reduce Cr(Ⅵ)to Cr(Ⅲ).
基金supported by the Preventive medicine and public health research project of Anhui,China(No.2011Y0103)the Natural Science Foundation of Anhui,China(No.11040606M216)
文摘To establish an analytical method for determination of four bisphenols (BPA, BPB, BPF, and BPS) and two alkylphenols (4-n-OP, 4-n-NP) in water by ultra performance liquid chromatography- tandem mass spectrometry (UPLC/MS/MS). The water samples were extracted and condensed with solid-phase extraction (SPE) using C18 cartridges and eluted by acetonitrile. Separation was carried out with Acquity BEH C8 column and detection were performed by UPLC/MS/MS. Quantification was calculated by using the internal standard BPA-d16 and 4-n-NP-d8. The linear correlation coefficients of these compounds in the range of 1.0-100.0μg/L were all over 0.999. The minimum detectable concentrations were 0.75-1.0 ng/L, and the recoveries ranged from 87.0% to 106.9%.
基金Project supported by the National Natural Science Foundation (Grant Nos 50532090,60606023 and 60621091)the Ministry of Science and Technology of China (Grant Nos 2002CB613502 and 2007CB936203)Australia Research Council
文摘A single crystalline Mg2Si film was formed by solid phase reaction (SPR) of a Si(111) substrate with an Mg overlayer capped with an oxide layer(s),which was enhanced by post annealing from room temperature to 100℃ in a molecular beam epitaxy (MBE) system.The thermal stability of the Mg2Si film was then systematically investigated by post annealing in an oxygen-radical ambient at 300℃,450℃ and 650℃,respectively.The Mg2Si film stayed stable until the annealing temperature reached 450℃ then it transformed into amorphous MgOx attributed to the decomposition of Mg2Si and the oxidization of dissociated Mg.
文摘A procedure for the preconcentration of copper was described in this paper using multi-walled carbon nanotubes (MWCNTs) oxidized by potassium permanganate as the adsorbent for the enrichment of trace copper in water samples. Important parameters, such as the sample pH, the concentration and volume of eluent, sample flow rate and volume, and interference of coexisting ions, were investigated. The obtained results indicated that proposed method possessed an excellent analytical performance. The linear range, the detection limit, and precison (RSD) were 1–100 ng/mL (R(2) = 0.9993), 0.32 ng/mL and 2.88%, respectively. The results showed that copper could be adsorbed quantitatively on the pretreated MWCNTs with potassium permanganate, and proposed method was very useful in the monitoring of copper in the environment.
文摘Base on the previous work in laboratory, a novel polyaniline doped with polydimethylsiloxane coating was developed on a stainless steel wire for solid phase microextraction(SPME) by electroplating method. This electroplating method not only has advantages of ease preparation and simple equipments required, but also increases the lifetime of the SPME fiber. The composite fiber(polyaniline/ polydimethylsiloxane(PANI/PDMS)) was evaluated by analyzing n-tridecane, n-tetradecane and n-pentadecane in aqueous sample. The new fiber coating showed comprehensive abilities to extract alkanes compounds. The relative standard deviations were found to be 6.8%-10.33%.
文摘Human urotension-Ⅱ was synthesized efficiently on Wang resin under microwave irradiation using Fmoc/tBu orthogonal protection strategy. Disulphide bridge was formed on solid phase with the irradiation of microwave, then the whole peptide was cleaved from the resin. The purity of crude peptide cyclized under microwave irradiation was higher than that under room temperature.
基金Supported by the Foundation of State Tabacco Monopoly Bureau(China) in Research Project(No.110200902008)
文摘The comparison of solid phase extraction(SPE) for the preconcentration and isolation of polyphenols in tobacco samples was carried out by ultra-high performance liquid chromatography/tandem mass spectrometry (UPLC/MS/MS) and multivariate analysis.Several adsorbing materials of SPE(C18,NH2,SAX and OASIS) were investigated.It was found that the C18 and OASIS cartridges can not only speed up the purification process,but also simplify the SPE operation.A UPLC/MS/MS was used for the determination of polyphenols in tobacco samples after purification.All analytes were separated and determined in 2min.The limit of detection was 0.05 ng/mL.Cluster analysis(CA) and principal component analysis(PCA) were used for the analysis of 4 varieties(flue-cured tobacco,oriental tobacco,sun-cured tobacco and burley) in order to interpret the effect of planting and machining process on the concentration of polyphenols.The different types of tobacco samples could be easily clustered by CA.PCA on the chemical composition of tobacco resulted in two principal components(PCs) that take 84.2% of the total variance.The PCA and CA indicate that the polyphenols can be used for distinguishing tobacco types.
基金grants from the Advanced Research Projects Agency (MDA-972-9l-J1013, N000l4-90-2032) and the World Health Organization (WHO 940l
文摘In order to accelerate the development of relatively inexpensive antimalarials that are effective against chloroquine-resistant strains of Plasmodium falciparum, a methodology for the solid phase synthesis of chalcone (1, 3-diphenyl-2-propen-1-one) analogues in reasonably high yields has been developed.
文摘A solid phase extraction procedure of methomyl and thiodicarb from environmental water was presented. This method utilizes a 40—60 mesh activated carbon cartridge and high performance liquid chromatography (HPLC). The 40—60 mesh activated carbon works faster and yield higher adsorption efficiency. Detection limits of methomyl and thiodicarb in environmental water are 0 1 μg/L and 0 2 μg/L, respectively. Average recoveries of fortified methomyl and thiodicarb in water are in the range of 90 7%—98 8% and 88 9%—103 6%, respectively. The relative standard deviations are lower than 7%. This method is simple, rapid, accurate and precise.