The measurement uncertainty provides complete information about an analytical result. This is very important because several decisions of compliance or non-compliance are based on analytical results in pharmaceutical ...The measurement uncertainty provides complete information about an analytical result. This is very important because several decisions of compliance or non-compliance are based on analytical results in pharmaceutical industries. The aim of this work was to evaluate and discuss the estimation of uncertainty in pharmaceutical analysis. The uncertainty is a useful tool in the assessment of compliance or non-compliance of in-process and final pharmaceutical products as well as in the assessment of pharmaceutical equivalence and stability study of drug products.展开更多
Fluorescent nanoparticles have good chemical stability and photostability,controllable optical properties and larger stokes shift.In light of their designability and functionability,the fluorescent nanoparticles are w...Fluorescent nanoparticles have good chemical stability and photostability,controllable optical properties and larger stokes shift.In light of their designability and functionability,the fluorescent nanoparticles are widely used as the fluorescent probes for diverse applications.To enhance the sensitivity and selectivity,the combination of the fluorescent nanoparticles with the molecularly imprinted polymer,i.e.molecularly imprinted fluorescent nanoparticles(MIFN),was an effective way.The sensor based on MIFN(the MIFN sensor)could be more compatible with the complex sample matrix,which was especially widely adopted in medical and biological analysis.In this mini-review,the construction method,detective mechanism and types of MIFN sensors are elaborated.The current applications of MIFN sensors in pharmaceutical analysis,including pesticides/herbicide,veterinary drugs/drugs residues and human related proteins,are highlighted based on the literature in the recent three years.Finally,the research prospect and development trend of the MIFN sensor are forecasted.展开更多
The year of 2017 is of historic importance for China. It was the year that China started to step into New Period. It was also the year that I had joined Wuhan University as a Luojia professor and set up my research gr...The year of 2017 is of historic importance for China. It was the year that China started to step into New Period. It was also the year that I had joined Wuhan University as a Luojia professor and set up my research group for ten years since I came back to China from University of Notre Dame, United States in 2007.展开更多
Objective: to analyze the adverse reactions caused by amoxicillin related drugs. Methods: 70 patients with adverse reactions caused by amoxicillin related drugs admitted to our hospital from October 2020 to October 20...Objective: to analyze the adverse reactions caused by amoxicillin related drugs. Methods: 70 patients with adverse reactions caused by amoxicillin related drugs admitted to our hospital from October 2020 to October 2021 were selected as the research objects, and the adverse reactions of all patients were statistically analyzed according to the route of administration and type of adverse reactions. Results: the probability of adr induced by intravenous drip was significantly higher than that of other routes, and the difference was statistically significant (P < 0.05). The occurrence probability of gastrointestinal adverse reactions was significantly higher than that of other adverse reactions, and the difference was statistically significant (P < 0.05). Conclusion: amoxicillin, as a kind of commonly used antibiotic drugs in the clinic has a very rich experience in practical use, but in the actual use also should fully consider the various factors, in this article can be found in the study, the occurrence of adverse reactions and drug delivery way of existence is very closely linked, therefore should according to patients condition when using using the most appropriate method, In order to reduce and prevent the occurrence of adverse reactions. At the same time, because the type of adverse reactions with the highest incidence is gastrointestinal adverse reactions, attention should be paid to the prevention of gastrointestinal adverse reactions when using drugs for patients, so as to greatly reduce the occurrence of gastrointestinal adverse reactions, give patients a higher guarantee of life safety, and lay a good foundation for faster recovery.展开更多
Monitoring critical quality attributes in pharmaceutical manufacturing ensures that the final product meets specified requirements.Process analysis allows for appropriate modifications and customization of pharmaceuti...Monitoring critical quality attributes in pharmaceutical manufacturing ensures that the final product meets specified requirements.Process analysis allows for appropriate modifications and customization of pharmaceutical design from formulation to production.The laborious sample presentation and throughput have stimulated the development of in-process spectroscopy methods for pharmaceutical analysis.Raman spectroscopy has demonstrated the unique advantages of rapid and nondestructive analysis,good interpretability,and effective moisture interference avoidance.The Raman imaging technique can obtain spatial and chemical information that is useful for characterizing drug quality.This article describes the applications of Raman spectroscopy and imaging techniques in pharmaceutical analysis.It covers the monitoring of crystal forms and particle size distribution,quantification of active pharmaceutical ingredients,evaluation of contents uniformity,prediction of dissolution profiles in solid preparations,identification of counterfeit drugs,and applications in reverse engineering and process analytical technology.Moreover,the challenges and prospects are proposed to facilitate the continued development of Raman spectroscopy and imaging techniques,providing necessary references for further research in this field.展开更多
Covalent organic frameworks(COFs)have numerous advantages,including high specific surface area,good stability,and ease of modification.These features have generated significant interest in utilizing COFs as chromatogr...Covalent organic frameworks(COFs)have numerous advantages,including high specific surface area,good stability,and ease of modification.These features have generated significant interest in utilizing COFs as chromatographic stationary phase materials.Herein,two monomers,1,3,5-tris-(4-aminophenyl)triazine(TAPT)and 1,3,5-benzenetricarboxaldehyde,are selected to construct the COF material.A novel core-shell type composite material named SiO_(2)@COF was prepared with the covalent triazine framework layer grafted on the silica by in situ growth method,and then the C18 chain was post-modifi ed on the SiO_(2)@COF material,named SiO_(2)@COF-C18.Multiple methods have been employed to illustrate the morphological and structural characteristics of the SiO_(2)@COF-C18 material.Then,several analytes,including anilines,polycyclic aromatic hydrocarbons(PAHs),alkylbenzenes,and positional isomers,were selected to study the separation mechanism of the SiO_(2)@COF-C18 column,which demonstrated that these analytes were separated on the SiO_(2)@COF-C18 column under chromatographic modes of hydrophobic interaction,π-πinteraction,steric hindrance eff ect,etc.The prepared chromatographic column had excellent repeatability and high separation efficiency,and it was used to determine acetaminophen tablets under reversed-phase conditions.These results open a new avenue for the post-modification of hydrophobic groups on COF materials for pharmaceutical analysis.展开更多
A new electrochemical method for the on-line determination of vitamin B1 is presented. Based on dead-stop endpoint biamperometry by using two platinum foil electrodes with an applied potential difference of 150 mV, vi...A new electrochemical method for the on-line determination of vitamin B1 is presented. Based on dead-stop endpoint biamperometry by using two platinum foil electrodes with an applied potential difference of 150 mV, vitamin B1 can be oxidized by hexacyanoferrate （ Ⅲ ） in a sodium hydroxide medium via a reversible indicating couple Fe（ CN）6^4- /Fe（CN）6^3- The cell current is linear with the concentration of vitamin B1 in the concentration range of 4. 0 × 10^-6-1.0 × 10^ -3 mol/L with a detection limit of 8.0 ×10 ^-7 mol/L（0. 27 μg/mL）. Most familiar excipients, ions and vitamins do not interfere with the determination of vitamin B1. The method displays the advantages of simplicity, high efficiency（ 180 samples/h）, and high selectivity, and is suitable for the determination of vitamin B1 in pharmaceutical preparations.展开更多
Similar to blood,interstitial fluid(ISF)contains exogenous drugs and biomarkers and may therefore substitute blood in drug analysis.However,current ISF extraction techniques require bulky instruments and are both time...Similar to blood,interstitial fluid(ISF)contains exogenous drugs and biomarkers and may therefore substitute blood in drug analysis.However,current ISF extraction techniques require bulky instruments and are both time-consuming and complicated,which has inspired the development of viable alternatives such as those relying on skin or tissue puncturing with microneedles.Currently,microneedles are widely employed for transdermal drug delivery and have been successfully used for ISF extraction by different mechanisms to facilitate subsequent analysis.The integration of microneedles with sensors enables in situ ISF analysis and specific compound monitoring,while the integration of monitoring and delivery functions in wearable devices allows real-time dose modification.Herein,we review the progress in drug analysis based on microneedle-assisted ISF extraction and discuss the related future opportunities and challenges.展开更多
A simple and selective micellar electrokinetic chromatographic （MEKC） method has been developed for the analysis of five pharmaceutical binary mixtures containing three non-steroidal antiinflammatory drugs （NSAIDs...A simple and selective micellar electrokinetic chromatographic （MEKC） method has been developed for the analysis of five pharmaceutical binary mixtures containing three non-steroidal antiinflammatory drugs （NSAIDs）. The investigated mixtures were Ibuprofen （IP）-Paracetamol （PC）, Ibuprofen （IP）-Chlorzoxazone （CZ）, Ibuprofen （IP）Methocarbamol （MC）, Ketoprofen （KP） Chlorzoxazone （CZ） and Diclofenac sodium （DS）-Lidocaine hydrochloride （LC）. The separation was run for all mixtures using borate buffer （20 mM, pH 9） containing 15% （v/v） methanol and 100 mM sodium dodecyl sulphate （SDS） at 15 kV and the components were detected at 214 nm. Different factors affecting the electrophoretic mobility of the seven investigated drugs were studied and optimized. The method was validated according to international conference of harmonization （ICH） guidelines and United States pharmacopoeia （USP）. The method was applied to the analysis of five pharmaceutical binary mixtures in their dosage forms. The results were compared with other reported high performance liquid chromatographic methods and no significant differences were observed.展开更多
Spectrophotometric method has been developed for the direct quantitative determination of captopril in pharmaceutical preparation and biological fluids （human plasma and urine） samples. The method was accomplished b...Spectrophotometric method has been developed for the direct quantitative determination of captopril in pharmaceutical preparation and biological fluids （human plasma and urine） samples. The method was accomplished based on parallel factor analysis （PARAFAC） and partial least squares （PLS）. The study was carried out in the pH range from 2.0 to 12.8 and with a concentration from 0.70 to 61.50μg mL^-1 of captopril. Multivariate calibration models such as PLS at various pH and PARAFAC were elaborated from ultraviolet spectra deconvolution and captopril determination. The best models for this system were obtained with PARAFAC and PLS at pH 2.0. The applications of the method for determination of real samples were evaluated by analysis of captopril in pharmaceutical preparations and biological fluids with satisfactory results. The accuracy of the method, evaluated through the RMSEE was 0.5801 for captopril with best calibration curve by PARAFAC and 0.6168 for captopril with PLS at pH 2.0 model.展开更多
Isoproterenol （ISPR） is an important catecholamine‐based drug that is widely used in the treatment of heart disease. However, overdose of this drug is very dangerous to the human body. In this study, a new sensor b...Isoproterenol （ISPR） is an important catecholamine‐based drug that is widely used in the treatment of heart disease. However, overdose of this drug is very dangerous to the human body. In this study, a new sensor based on a pyrogallol red modified‐multiwalled carbon nanotube paste electrode （PGRMMWCNTPE） was prepared and used for high sensitivity determination of ISPR in aqueous solution. Electrocatalytic oxidation of ISPR at the PGRMMWCNTPE was investigated by chronoam‐perometry, cyclic voltammetry, and square‐wave voltammetry. The values of the catalytic rate con‐stant, electron transfer coefficient, and diffusion coefficient for ISPR oxidation were then calculated using voltammetric data. A linear calibration curve was constructed for ISPR concentration in the range 0.8–570μmol/L with a detection limit of 0.47μmol/L ISPR. The sensor was then applied to the determination of ISPR in urine and drug samples with satisfactory results.展开更多
The characteristics, performance and application of membrane electrode based on ion associate of diclofenac with base dye Safranine T are described. The electrode response to diclofenac has the sensitivity of 47 ±...The characteristics, performance and application of membrane electrode based on ion associate of diclofenac with base dye Safranine T are described. The electrode response to diclofenac has the sensitivity of 47 ± 1.0 mV decade(?1) over the range of 5 × 10(?5) to 5 × 10(?2) mol/L at pH 6–12, and the detection limit of 3.2 × 10(?5) mol/L. The electrode is easy assembled at a relatively low cost has fast response time (2–4 s) and can be used for a period up to 3.5 months without any considerable divergence in potential. The proposed sensor displayed good selectivity for diclofenac in the presence of different substances. It was used to determine diclofenac in pharmaceuticals by means of the standard addition method.展开更多
Designing three-dimensional(3D)catalytic sites in single-atom catalysts(SACs)that mimic thyroid peroxidase(TPO)function for achieving iodotyrosine coupling,although highly desirable for the synthesis of thyroid hormon...Designing three-dimensional(3D)catalytic sites in single-atom catalysts(SACs)that mimic thyroid peroxidase(TPO)function for achieving iodotyrosine coupling,although highly desirable for the synthesis of thyroid hormones,poses a great challenge.Herein,we design and synthesize a class of SACs with 3D catalytic centers composed of Cu-N_(5)as catalytic sites and BO_(2) as binding sites(BO_(2)/Cu N_(5)C)for mimicking TPO in activating H_(2)O_(2) to facilitate tyrosine iodination and conjugation for producing thyroid hormones.We demonstrate that the as-prepared BO_(2)/Cu N_(5)C not only provides binding sites for H_(2)O_(2) through hydrogen bond interactions but also possesses catalytic sites to promote an alternative O–O heterolysis process.BO_(2)/Cu N_(5)C with TPO-like catalytic centers can produce 3,3′,5-triiodothyronine and D-thyroxine with 2.4-fold and 11.1-fold improvements relative to those of Cu N_(5)C.Besides,the assessment of 2-mercapto-1-methylimidazole and 6-propyl-2-thiouracil in vitro investigations of antithyroid drugs corresponds well with the European Thyroid Association guidelines and therefore can provide clinical medication guidance to prevent toxic reactions.Overall,this work unlocks an approach to precisely simulate the natural enzyme active site for amino acid coupling and pharmaceutical assessment.展开更多
A simple, rapid and sensitive flow injection chemiluminescence （FI-CL） method has been developed for the determination of meloxicam. The method is based on the CL-emitting reaction between meloxicam and potassium pe...A simple, rapid and sensitive flow injection chemiluminescence （FI-CL） method has been developed for the determination of meloxicam. The method is based on the CL-emitting reaction between meloxicam and potassium permanganate in a hydrochloric acid medium, enhanced by formaldehyde （HCHO）. Under optimum conditions, calibration curve over the range of 1.0-20.0μg/mL was obtained. The proposed method was successfully applied to the determination of meloxicam in capsules with no evi- dence of interference from common excipients. The detection limit of this method was 25.6 ng/mL. The relative standard deviation was 2.1% for 10.0 μg/mL meloxicam. The sample throughput was found to be 120 samples/h.展开更多
Fluorescence characteristics of complex system of rare earth terbium （Tb3＋）, norfloxacin, 1,10-phenanthroline（1,10-phen） and sur- factant sodium dodecyl benzene sulfonate （SDBS） had been studied by using fluore...Fluorescence characteristics of complex system of rare earth terbium （Tb3＋）, norfloxacin, 1,10-phenanthroline（1,10-phen） and sur- factant sodium dodecyl benzene sulfonate （SDBS） had been studied by using fluorescence spectroscopy. In a buffer solution （pH=6.3）, the fluorescence intensity of the norfloxacin-Tb3＋ （NFLX-Tb3＋） system had been remarkably enhanced by SDBS and 1,10-Phen. When excited at 335 nm, a good linear relationship between fluorescence intensity of NFLX-Tb3＋ system and NFLX concentration was obtained in the range of 8× 10-8-4× 10-6 mol/L, and the linear equation was F=2× 10^8 CNFLX＋22.7 with correlation coefficient of 0.9959. In addition, this method was compared with some previous literatures, the proposed method had relatively higher sensitivity and lower detect limit. The method was sim- ple, rapid, sensitive, practical and suitable for direct analysis of pharmaceutical preparation. It was successfully applied to determine the cap- sules, human serum and urine in real pharmaceutical samples.展开更多
Aim To develop a simple and specific high-performance liquid chromatographic(HPLC) method, suitable for the pharmacokinetic studies in vivo, to determine the concentrations of2-amino-6-cyclopropylamino-9-(2,3-dideoxy-...Aim To develop a simple and specific high-performance liquid chromatographic(HPLC) method, suitable for the pharmacokinetic studies in vivo, to determine the concentrations of2-amino-6-cyclopropylamino-9-(2,3-dideoxy-β-D-glyceropent-2-enofuranosyl)purine (Cyclo-D4G, IMGprodrug) in rat plasma, urine and liver homogenates. Methods Chromatography was performed with C-18Hypersil ODS column and a mobile phase of 7% (v/v) acetonitrile in phosphate buffer, pH 7.40, withUV detection at 283 nm. Results The average extraction recovery of Cyclo-D4G in rat plasma and urinewas 100.1% over its linear range of 0.5 - 80 μg·mL^(-1). The accuracy of the assay was 99.4% .The intra-and inter-day RSDs were less than 9.0% . Conclusion The analytical method was found to beapplicable, reliable and suitable for pharmacokinetic studies.展开更多
A simple and highly sensitive method for the determination of triamcinolone acetonide in pharmaceutical formulations is presented.The approach is based on the fluorescence of production of triamcinolone acetonide oxid...A simple and highly sensitive method for the determination of triamcinolone acetonide in pharmaceutical formulations is presented.The approach is based on the fluorescence of production of triamcinolone acetonide oxidized by concentrated sulfuric acid.The effect of H2SO4,β-cyclodextrin(β-CD),solvent and cetyltrimethylammonium bromide(CTMAB)were discussed.And two analytical systems were established.One is CTMAB system,the linear range is 0–4.6×10^(-6)mol/L,and the detection limit is 3.59×10^(-8)mol/L.The other isβ-CD and ethanol system,the linear range is 0–2.3×10^(-6)mol/L and the detection limit is 1.91×10^(-8)mol/L.The selectivity of analysis,the analytical figures of optimization,and the accuracy of the method are demonstrated with the determination of triamcinolone acetonide in pharmaceutical preparations.展开更多
A high-performance liquid chromatography method for the simultaneous determination of seven bioactive ginsenosides with diol stationary phase and isocratic elution was used to determin the ginsenosides in ginseng prod...A high-performance liquid chromatography method for the simultaneous determination of seven bioactive ginsenosides with diol stationary phase and isocratic elution was used to determin the ginsenosides in ginseng products. The optimization of the chromatographic separation was performed and the effect of temperature on separation was investigated. Using the validated procedure, the developed method was demonstrated to be more sensitive and effective than the conventional reversed-phase chromatography, where the chromatographic run is time-consuming to analyze a large number of ginsenosides. The results indicated that the developed method can be used for the quantitative determination of ginsenosides in complex ginseng samples.展开更多
The electrochemical oxidation behavior and voltammetric assay of gemifloxacin were investigated using differential-pulse and cyclic voltammetry on a screen-printed carbon electrode.The effects of pH,scan rates,and con...The electrochemical oxidation behavior and voltammetric assay of gemifloxacin were investigated using differential-pulse and cyclic voltammetry on a screen-printed carbon electrode.The effects of pH,scan rates,and concentration of the drug on the anodic peak current were studied.Voltammograms of gemifloxacin in Tris-HCl buffer（pH 7.0） exhibited a well-defined single oxidation peak.A differential-pulse voltammetric procedure for the quantitation of gemifloxacin has been developed and suitably validated with respect to linearity,limits of detection and quantification,accuracy,precision,specificity,and robustness.The calibration was linear from 0.5 to 10.0 μM,and the limits of detection and quantification were 0.15 and 5.0 μM.Recoveries ranging from 96.26% to 103.64% were obtained.The method was successfully applied to the determination of gemifloxacin in pharmaceutical tablets without any pre-treatment.Excipients present in the tablets did not interfere in the assay.展开更多
A novel electrogenerated chemiluminescence(ECL)sensor for the determination of metoclopramide was developed by employing ruthenium complex as an ECL signal producer and an ordered mesoporous carbon(OMC)material as mod...A novel electrogenerated chemiluminescence(ECL)sensor for the determination of metoclopramide was developed by employing ruthenium complex as an ECL signal producer and an ordered mesoporous carbon(OMC)material as modified material.The ECL sensor was fabricated by adsorption ruthenium complex into a mixture of OMC and Nafion,which showed good electrochemical and ECL behaviors.It was found that the ECL intensity of the sensor fabricated was greatly enhanced in the presence of metoclopramide.Based on this finding,a highly sensitive and reproducible ECL method was developed for the determination of metoclopramide.The result showed that the ECL intensity was linear with the concentration of metoclopramide in the range from 1.0×10-10 to 5.0×10-7M and the detection limit was 3×10-11M.The ECL sensor exhibited a long-term stability and a fine reproducibility with relative standard deviation of 1.0 % for 1.0×10-10M metoclopramide in 18 continuous determinations.The developed method has been applied to the determination of metoclopramide in tablet samples with satisfactory results.展开更多
基金supported by Fundacao de Apoio à Pesquisa do Estado de Sao Paulo(FAPESP)
文摘The measurement uncertainty provides complete information about an analytical result. This is very important because several decisions of compliance or non-compliance are based on analytical results in pharmaceutical industries. The aim of this work was to evaluate and discuss the estimation of uncertainty in pharmaceutical analysis. The uncertainty is a useful tool in the assessment of compliance or non-compliance of in-process and final pharmaceutical products as well as in the assessment of pharmaceutical equivalence and stability study of drug products.
基金This work is supported by the National Natural Science Foundation of China(No.21804105)by the Fundamental Research Funds for the Central Universities(No.5003515037)supported by the Huazhong University of Science and Technology Start-up Fund to Xu YU.
文摘Fluorescent nanoparticles have good chemical stability and photostability,controllable optical properties and larger stokes shift.In light of their designability and functionability,the fluorescent nanoparticles are widely used as the fluorescent probes for diverse applications.To enhance the sensitivity and selectivity,the combination of the fluorescent nanoparticles with the molecularly imprinted polymer,i.e.molecularly imprinted fluorescent nanoparticles(MIFN),was an effective way.The sensor based on MIFN(the MIFN sensor)could be more compatible with the complex sample matrix,which was especially widely adopted in medical and biological analysis.In this mini-review,the construction method,detective mechanism and types of MIFN sensors are elaborated.The current applications of MIFN sensors in pharmaceutical analysis,including pesticides/herbicide,veterinary drugs/drugs residues and human related proteins,are highlighted based on the literature in the recent three years.Finally,the research prospect and development trend of the MIFN sensor are forecasted.
文摘The year of 2017 is of historic importance for China. It was the year that China started to step into New Period. It was also the year that I had joined Wuhan University as a Luojia professor and set up my research group for ten years since I came back to China from University of Notre Dame, United States in 2007.
文摘Objective: to analyze the adverse reactions caused by amoxicillin related drugs. Methods: 70 patients with adverse reactions caused by amoxicillin related drugs admitted to our hospital from October 2020 to October 2021 were selected as the research objects, and the adverse reactions of all patients were statistically analyzed according to the route of administration and type of adverse reactions. Results: the probability of adr induced by intravenous drip was significantly higher than that of other routes, and the difference was statistically significant (P < 0.05). The occurrence probability of gastrointestinal adverse reactions was significantly higher than that of other adverse reactions, and the difference was statistically significant (P < 0.05). Conclusion: amoxicillin, as a kind of commonly used antibiotic drugs in the clinic has a very rich experience in practical use, but in the actual use also should fully consider the various factors, in this article can be found in the study, the occurrence of adverse reactions and drug delivery way of existence is very closely linked, therefore should according to patients condition when using using the most appropriate method, In order to reduce and prevent the occurrence of adverse reactions. At the same time, because the type of adverse reactions with the highest incidence is gastrointestinal adverse reactions, attention should be paid to the prevention of gastrointestinal adverse reactions when using drugs for patients, so as to greatly reduce the occurrence of gastrointestinal adverse reactions, give patients a higher guarantee of life safety, and lay a good foundation for faster recovery.
基金financial support of Key Project of Tianjin Natural Science Foundation(23JCZDJC00720)S&T Project of Haihe Laboratory of Modern Chinese Medicine(22HHZYSS00004)+1 种基金the Key University Science Research Project of Anhui Province(KJ2021A1146,KJ2020A0775)first batch of provincial science and technology mission projects in Anhui Province(2023tpt014)。
文摘Monitoring critical quality attributes in pharmaceutical manufacturing ensures that the final product meets specified requirements.Process analysis allows for appropriate modifications and customization of pharmaceutical design from formulation to production.The laborious sample presentation and throughput have stimulated the development of in-process spectroscopy methods for pharmaceutical analysis.Raman spectroscopy has demonstrated the unique advantages of rapid and nondestructive analysis,good interpretability,and effective moisture interference avoidance.The Raman imaging technique can obtain spatial and chemical information that is useful for characterizing drug quality.This article describes the applications of Raman spectroscopy and imaging techniques in pharmaceutical analysis.It covers the monitoring of crystal forms and particle size distribution,quantification of active pharmaceutical ingredients,evaluation of contents uniformity,prediction of dissolution profiles in solid preparations,identification of counterfeit drugs,and applications in reverse engineering and process analytical technology.Moreover,the challenges and prospects are proposed to facilitate the continued development of Raman spectroscopy and imaging techniques,providing necessary references for further research in this field.
基金the Project of Sichuan Department of Science and Technology(2022NSFSC0622)the Scientifi c Research Project of Southwest Medical University(2021ZKMS043)+1 种基金the Science and Technology Project of Luzhou(2021-JYJ-74)the National Natural Science Foundation of China(21974015)。
文摘Covalent organic frameworks(COFs)have numerous advantages,including high specific surface area,good stability,and ease of modification.These features have generated significant interest in utilizing COFs as chromatographic stationary phase materials.Herein,two monomers,1,3,5-tris-(4-aminophenyl)triazine(TAPT)and 1,3,5-benzenetricarboxaldehyde,are selected to construct the COF material.A novel core-shell type composite material named SiO_(2)@COF was prepared with the covalent triazine framework layer grafted on the silica by in situ growth method,and then the C18 chain was post-modifi ed on the SiO_(2)@COF material,named SiO_(2)@COF-C18.Multiple methods have been employed to illustrate the morphological and structural characteristics of the SiO_(2)@COF-C18 material.Then,several analytes,including anilines,polycyclic aromatic hydrocarbons(PAHs),alkylbenzenes,and positional isomers,were selected to study the separation mechanism of the SiO_(2)@COF-C18 column,which demonstrated that these analytes were separated on the SiO_(2)@COF-C18 column under chromatographic modes of hydrophobic interaction,π-πinteraction,steric hindrance eff ect,etc.The prepared chromatographic column had excellent repeatability and high separation efficiency,and it was used to determine acetaminophen tablets under reversed-phase conditions.These results open a new avenue for the post-modification of hydrophobic groups on COF materials for pharmaceutical analysis.
文摘A new electrochemical method for the on-line determination of vitamin B1 is presented. Based on dead-stop endpoint biamperometry by using two platinum foil electrodes with an applied potential difference of 150 mV, vitamin B1 can be oxidized by hexacyanoferrate （ Ⅲ ） in a sodium hydroxide medium via a reversible indicating couple Fe（ CN）6^4- /Fe（CN）6^3- The cell current is linear with the concentration of vitamin B1 in the concentration range of 4. 0 × 10^-6-1.0 × 10^ -3 mol/L with a detection limit of 8.0 ×10 ^-7 mol/L（0. 27 μg/mL）. Most familiar excipients, ions and vitamins do not interfere with the determination of vitamin B1. The method displays the advantages of simplicity, high efficiency（ 180 samples/h）, and high selectivity, and is suitable for the determination of vitamin B1 in pharmaceutical preparations.
基金the National Natural Science Foundation of China(Grant No.:82074031)the Program for Professor of Special Appointment(Eastern Scholar)at Shanghai Institutions of Higher Learning(Grant No.:TP2020054)China,and Program for Shanghai High-level Local University Innovation Team(Grant No.:SZY20220315),China.
文摘Similar to blood,interstitial fluid(ISF)contains exogenous drugs and biomarkers and may therefore substitute blood in drug analysis.However,current ISF extraction techniques require bulky instruments and are both time-consuming and complicated,which has inspired the development of viable alternatives such as those relying on skin or tissue puncturing with microneedles.Currently,microneedles are widely employed for transdermal drug delivery and have been successfully used for ISF extraction by different mechanisms to facilitate subsequent analysis.The integration of microneedles with sensors enables in situ ISF analysis and specific compound monitoring,while the integration of monitoring and delivery functions in wearable devices allows real-time dose modification.Herein,we review the progress in drug analysis based on microneedle-assisted ISF extraction and discuss the related future opportunities and challenges.
文摘A simple and selective micellar electrokinetic chromatographic （MEKC） method has been developed for the analysis of five pharmaceutical binary mixtures containing three non-steroidal antiinflammatory drugs （NSAIDs）. The investigated mixtures were Ibuprofen （IP）-Paracetamol （PC）, Ibuprofen （IP）-Chlorzoxazone （CZ）, Ibuprofen （IP）Methocarbamol （MC）, Ketoprofen （KP） Chlorzoxazone （CZ） and Diclofenac sodium （DS）-Lidocaine hydrochloride （LC）. The separation was run for all mixtures using borate buffer （20 mM, pH 9） containing 15% （v/v） methanol and 100 mM sodium dodecyl sulphate （SDS） at 15 kV and the components were detected at 214 nm. Different factors affecting the electrophoretic mobility of the seven investigated drugs were studied and optimized. The method was validated according to international conference of harmonization （ICH） guidelines and United States pharmacopoeia （USP）. The method was applied to the analysis of five pharmaceutical binary mixtures in their dosage forms. The results were compared with other reported high performance liquid chromatographic methods and no significant differences were observed.
文摘Spectrophotometric method has been developed for the direct quantitative determination of captopril in pharmaceutical preparation and biological fluids （human plasma and urine） samples. The method was accomplished based on parallel factor analysis （PARAFAC） and partial least squares （PLS）. The study was carried out in the pH range from 2.0 to 12.8 and with a concentration from 0.70 to 61.50μg mL^-1 of captopril. Multivariate calibration models such as PLS at various pH and PARAFAC were elaborated from ultraviolet spectra deconvolution and captopril determination. The best models for this system were obtained with PARAFAC and PLS at pH 2.0. The applications of the method for determination of real samples were evaluated by analysis of captopril in pharmaceutical preparations and biological fluids with satisfactory results. The accuracy of the method, evaluated through the RMSEE was 0.5801 for captopril with best calibration curve by PARAFAC and 0.6168 for captopril with PLS at pH 2.0 model.
基金Majlesi Branch, Islamic Azad University, for their support
文摘Isoproterenol （ISPR） is an important catecholamine‐based drug that is widely used in the treatment of heart disease. However, overdose of this drug is very dangerous to the human body. In this study, a new sensor based on a pyrogallol red modified‐multiwalled carbon nanotube paste electrode （PGRMMWCNTPE） was prepared and used for high sensitivity determination of ISPR in aqueous solution. Electrocatalytic oxidation of ISPR at the PGRMMWCNTPE was investigated by chronoam‐perometry, cyclic voltammetry, and square‐wave voltammetry. The values of the catalytic rate con‐stant, electron transfer coefficient, and diffusion coefficient for ISPR oxidation were then calculated using voltammetric data. A linear calibration curve was constructed for ISPR concentration in the range 0.8–570μmol/L with a detection limit of 0.47μmol/L ISPR. The sensor was then applied to the determination of ISPR in urine and drug samples with satisfactory results.
文摘The characteristics, performance and application of membrane electrode based on ion associate of diclofenac with base dye Safranine T are described. The electrode response to diclofenac has the sensitivity of 47 ± 1.0 mV decade(?1) over the range of 5 × 10(?5) to 5 × 10(?2) mol/L at pH 6–12, and the detection limit of 3.2 × 10(?5) mol/L. The electrode is easy assembled at a relatively low cost has fast response time (2–4 s) and can be used for a period up to 3.5 months without any considerable divergence in potential. The proposed sensor displayed good selectivity for diclofenac in the presence of different substances. It was used to determine diclofenac in pharmaceuticals by means of the standard addition method.
基金the financial support of the National Natural Science Foundation of China(22127803,22174110,52470193,and 22304096)the Nature Science Foundation of Shandong Provinces(ZR2023QB006)+1 种基金the project funded by China Postdoctoral Science Foundation(2023M741853)the Plan for Youth Innovation Team of Colleges in Shandong Province。
文摘Designing three-dimensional(3D)catalytic sites in single-atom catalysts(SACs)that mimic thyroid peroxidase(TPO)function for achieving iodotyrosine coupling,although highly desirable for the synthesis of thyroid hormones,poses a great challenge.Herein,we design and synthesize a class of SACs with 3D catalytic centers composed of Cu-N_(5)as catalytic sites and BO_(2) as binding sites(BO_(2)/Cu N_(5)C)for mimicking TPO in activating H_(2)O_(2) to facilitate tyrosine iodination and conjugation for producing thyroid hormones.We demonstrate that the as-prepared BO_(2)/Cu N_(5)C not only provides binding sites for H_(2)O_(2) through hydrogen bond interactions but also possesses catalytic sites to promote an alternative O–O heterolysis process.BO_(2)/Cu N_(5)C with TPO-like catalytic centers can produce 3,3′,5-triiodothyronine and D-thyroxine with 2.4-fold and 11.1-fold improvements relative to those of Cu N_(5)C.Besides,the assessment of 2-mercapto-1-methylimidazole and 6-propyl-2-thiouracil in vitro investigations of antithyroid drugs corresponds well with the European Thyroid Association guidelines and therefore can provide clinical medication guidance to prevent toxic reactions.Overall,this work unlocks an approach to precisely simulate the natural enzyme active site for amino acid coupling and pharmaceutical assessment.
文摘A simple, rapid and sensitive flow injection chemiluminescence （FI-CL） method has been developed for the determination of meloxicam. The method is based on the CL-emitting reaction between meloxicam and potassium permanganate in a hydrochloric acid medium, enhanced by formaldehyde （HCHO）. Under optimum conditions, calibration curve over the range of 1.0-20.0μg/mL was obtained. The proposed method was successfully applied to the determination of meloxicam in capsules with no evi- dence of interference from common excipients. The detection limit of this method was 25.6 ng/mL. The relative standard deviation was 2.1% for 10.0 μg/mL meloxicam. The sample throughput was found to be 120 samples/h.
基金Project supported by National Natural Science Foundation of China(21003063)the Natural Science Foundation of Heilongjiang Province ofChina(B201006,B201015)+3 种基金Research Project of Heilongjiang Provincial Health Bureau of China(2012-263,2010-504)Chinese MedicineResearch Project of Heilongjiang Province(ZHY12-Z195)supported by the Scientific and Technical Research Project of Education Department of Heilongjiang Province(11551482)2012 Graduate Innovation Scientific Research Project Funds of Jiamusi University and Great Foster Projectof Jiamusi University(LZP2011-003)
文摘Fluorescence characteristics of complex system of rare earth terbium （Tb3＋）, norfloxacin, 1,10-phenanthroline（1,10-phen） and sur- factant sodium dodecyl benzene sulfonate （SDBS） had been studied by using fluorescence spectroscopy. In a buffer solution （pH=6.3）, the fluorescence intensity of the norfloxacin-Tb3＋ （NFLX-Tb3＋） system had been remarkably enhanced by SDBS and 1,10-Phen. When excited at 335 nm, a good linear relationship between fluorescence intensity of NFLX-Tb3＋ system and NFLX concentration was obtained in the range of 8× 10-8-4× 10-6 mol/L, and the linear equation was F=2× 10^8 CNFLX＋22.7 with correlation coefficient of 0.9959. In addition, this method was compared with some previous literatures, the proposed method had relatively higher sensitivity and lower detect limit. The method was sim- ple, rapid, sensitive, practical and suitable for direct analysis of pharmaceutical preparation. It was successfully applied to determine the cap- sules, human serum and urine in real pharmaceutical samples.
文摘Aim To develop a simple and specific high-performance liquid chromatographic(HPLC) method, suitable for the pharmacokinetic studies in vivo, to determine the concentrations of2-amino-6-cyclopropylamino-9-(2,3-dideoxy-β-D-glyceropent-2-enofuranosyl)purine (Cyclo-D4G, IMGprodrug) in rat plasma, urine and liver homogenates. Methods Chromatography was performed with C-18Hypersil ODS column and a mobile phase of 7% (v/v) acetonitrile in phosphate buffer, pH 7.40, withUV detection at 283 nm. Results The average extraction recovery of Cyclo-D4G in rat plasma and urinewas 100.1% over its linear range of 0.5 - 80 μg·mL^(-1). The accuracy of the assay was 99.4% .The intra-and inter-day RSDs were less than 9.0% . Conclusion The analytical method was found to beapplicable, reliable and suitable for pharmacokinetic studies.
基金Supported by the National Natural Science Foun-dation of China(20275028)
文摘A simple and highly sensitive method for the determination of triamcinolone acetonide in pharmaceutical formulations is presented.The approach is based on the fluorescence of production of triamcinolone acetonide oxidized by concentrated sulfuric acid.The effect of H2SO4,β-cyclodextrin(β-CD),solvent and cetyltrimethylammonium bromide(CTMAB)were discussed.And two analytical systems were established.One is CTMAB system,the linear range is 0–4.6×10^(-6)mol/L,and the detection limit is 3.59×10^(-8)mol/L.The other isβ-CD and ethanol system,the linear range is 0–2.3×10^(-6)mol/L and the detection limit is 1.91×10^(-8)mol/L.The selectivity of analysis,the analytical figures of optimization,and the accuracy of the method are demonstrated with the determination of triamcinolone acetonide in pharmaceutical preparations.
基金supported by the postdoctoral fellowship of Jilin Institute of Chemical Technology
文摘A high-performance liquid chromatography method for the simultaneous determination of seven bioactive ginsenosides with diol stationary phase and isocratic elution was used to determin the ginsenosides in ginseng products. The optimization of the chromatographic separation was performed and the effect of temperature on separation was investigated. Using the validated procedure, the developed method was demonstrated to be more sensitive and effective than the conventional reversed-phase chromatography, where the chromatographic run is time-consuming to analyze a large number of ginsenosides. The results indicated that the developed method can be used for the quantitative determination of ginsenosides in complex ginseng samples.
文摘The electrochemical oxidation behavior and voltammetric assay of gemifloxacin were investigated using differential-pulse and cyclic voltammetry on a screen-printed carbon electrode.The effects of pH,scan rates,and concentration of the drug on the anodic peak current were studied.Voltammograms of gemifloxacin in Tris-HCl buffer（pH 7.0） exhibited a well-defined single oxidation peak.A differential-pulse voltammetric procedure for the quantitation of gemifloxacin has been developed and suitably validated with respect to linearity,limits of detection and quantification,accuracy,precision,specificity,and robustness.The calibration was linear from 0.5 to 10.0 μM,and the limits of detection and quantification were 0.15 and 5.0 μM.Recoveries ranging from 96.26% to 103.64% were obtained.The method was successfully applied to the determination of gemifloxacin in pharmaceutical tablets without any pre-treatment.Excipients present in the tablets did not interfere in the assay.
基金supported by the National Natural Science Foundation of China(No.20805028)
文摘A novel electrogenerated chemiluminescence(ECL)sensor for the determination of metoclopramide was developed by employing ruthenium complex as an ECL signal producer and an ordered mesoporous carbon(OMC)material as modified material.The ECL sensor was fabricated by adsorption ruthenium complex into a mixture of OMC and Nafion,which showed good electrochemical and ECL behaviors.It was found that the ECL intensity of the sensor fabricated was greatly enhanced in the presence of metoclopramide.Based on this finding,a highly sensitive and reproducible ECL method was developed for the determination of metoclopramide.The result showed that the ECL intensity was linear with the concentration of metoclopramide in the range from 1.0×10-10 to 5.0×10-7M and the detection limit was 3×10-11M.The ECL sensor exhibited a long-term stability and a fine reproducibility with relative standard deviation of 1.0 % for 1.0×10-10M metoclopramide in 18 continuous determinations.The developed method has been applied to the determination of metoclopramide in tablet samples with satisfactory results.
