Analytical Chemistry Letters最新文献_第10页

The New RP-HPLC Method for Simultaneous Quantification of Cinnarizine, its Five Specified Impurities, Two Degradation Products with Two Antioxidants and Confirmation of all by HPLC-ESI-MS in Different Pharmaceutical Drug Formulations 采用反相高效液相色谱(RP-HPLC)同时定量测定不同制剂中肉桂碱、五种指定杂质、两种抗氧化剂降解产物，并采用HPLC-ESI-MS确认

Analytical Chemistry Letters Pub Date : 2022-05-04 DOI: 10.1080/22297928.2022.2067006

D. Mhaske, A. Kumbhar

{"title":"The New RP-HPLC Method for Simultaneous Quantification of Cinnarizine, its Five Specified Impurities, Two Degradation Products with Two Antioxidants and Confirmation of all by HPLC-ESI-MS in Different Pharmaceutical Drug Formulations","authors":"D. Mhaske, A. Kumbhar","doi":"10.1080/22297928.2022.2067006","DOIUrl":"https://doi.org/10.1080/22297928.2022.2067006","url":null,"abstract":"Abstract To determine the safety and efficacy, we have developed and validated the RP-HPLC method for simultaneous quantification of cinnarizine, its five specified impurities and two degradation products in cinnarizine API, tablets and capsules and including two antioxidants in an oral suspension formulation. The chromatographic separation was achieved in gradient elution mode with 1.00mL/min flow on an Ascentis Express C18 (150mm, 4.6mm and 2.7µm particle size) column at 40.0°C column temperature using 0.05% acetic acid in mixtures of 10mM ammonium acetate and acetonitrile. All peaks are eluted within 30 minutes with a 10µL injection volume and detected at a 230nm wavelength. The results of the validation of the proposed RP-HPLC method as per ICH guidelines revealed that the method is specific, accurate, precise, linear and robust for quantification purposes. The recoveries for all specified impurities, degradation products and cinnarizine at a lower concentration were found in the range of 100.0±10.0%. While the assay values were within 100.0±2.0% for cinnarizine and antioxidants (methylparaben and propylparaben). The LOD and LOQ were 0.1125µg/mL and 0.1875µg/mL, respectively. The linearity curves for all the ten analytes mentioned above showed good linearity (r≥0.999). This research work presents the first RP-HPLC method for simultaneous quantification of all ten analytes with unknown impurities, as well as an HPLC-ESI-MS method for correct identification and confirmation of results. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"8 1","pages":"391 - 408"},"PeriodicalIF":0.0,"publicationDate":"2022-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"84235504","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 1

Resolving Problems Encountered in Spectrophotometric Analysis of a Ternary Mixture of Linagliptin, Empagliflozin and Metformin Hydrochloride 利格列汀、恩格列净、盐酸二甲双胍三元混合物分光光度法分析中存在的问题

Analytical Chemistry Letters Pub Date : 2022-05-04 DOI: 10.1080/22297928.2022.2058414

Samar H. Elagamy

{"title":"Resolving Problems Encountered in Spectrophotometric Analysis of a Ternary Mixture of Linagliptin, Empagliflozin and Metformin Hydrochloride","authors":"Samar H. Elagamy","doi":"10.1080/22297928.2022.2058414","DOIUrl":"https://doi.org/10.1080/22297928.2022.2058414","url":null,"abstract":"Abstract There are two main problems encountered in spectrophotometric analysis of a ternary mixture composed of linagliptin LINA, empagliflozin EMPA and metformin hydrochloride MET. The first problem is due to the severe overlap in their zero and derivative spectra. To overcome this problem, LINA was determined by direct spectrophotometry at λ max = 298 nm where there is no interference from other components while, EMPA and MET were determined using double divisor ratio spectra derivative method DDRD. In this method, the first derivative spectra were calculated for ratio spectra generated by dividing the absorption spectra of ternary mixtures containing increasing concentrations of one of the components by a standard spectrum of binary mixture of the other two components (double divisor). The calibration graphs were constructed by measuring the amplitude at either the minimum or maximum wavelengths against the concentrations. The selected wavelengths for determination of EMPA and MET are 282.92 and 250 nm, respectively. The second problem arises from the presence of LINA and EMPA as minor components in their recently approved dosage form with MET thus, sample enrichment through spiking was employed for LINA and EMPA to enable their spectrophotometric analysis in laboratory prepared mixtures that have the same ratio of the three components as in their pharmaceutical dosage form. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"20 1","pages":"349 - 357"},"PeriodicalIF":0.0,"publicationDate":"2022-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77736689","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 1

PEG-400 Catalyzed N-C, O-C & C-S Bond Formations: A Robust Sonication Promoted Synthesis of Benzo[d]oxazole-2 (3H)-thione & Benzo[d]thiazole-2(3H)-thione Hybrids PEG-400催化的N-C, O-C和C-S键形成:一个稳健的超声催化合成苯并[d]恶唑-2(3H)-硫酮和苯并[d]噻唑-2(3H)-硫酮杂化物

Analytical Chemistry Letters Pub Date : 2022-05-04 DOI: 10.1080/22297928.2022.2068376

Aadil Yaseen, M. Waseem, Mahapara Qadir, P. Dar, Shariqah Hijazi, Mir Ashiq Hussain, W. A. Shah

引用次数: 0

Stochastic Dynamic Electrospray Ionization Mass Spectrometric Quantitative Analysis of Metronidazole in Human Urine 随机动态电喷雾电离质谱法定量分析人尿中甲硝唑

Analytical Chemistry Letters Pub Date : 2022-05-04 DOI: 10.1080/22297928.2022.2086822

B. Ivanova, M. Spiteller

{"title":"Stochastic Dynamic Electrospray Ionization Mass Spectrometric Quantitative Analysis of Metronidazole in Human Urine","authors":"B. Ivanova, M. Spiteller","doi":"10.1080/22297928.2022.2086822","DOIUrl":"https://doi.org/10.1080/22297928.2022.2086822","url":null,"abstract":"Abstract The study reports quantification of metronidazole (MTZ) in clinical human urine employing our innovative stochastic dynamic equation D”SD =2.6388.10-17.(–). There are direct analysis without presence of internal standard, using ultra-high accuracy nano-electrospray ionization (ESI) mass spectrometry (MS), quantum chemistry and chemometrics, respectively. The linear calibration D”SD =f(conc.) equations are obtained for concentration range 2.5 to 25000 ng.(mL)-1 of spiked urine samples, examining analyte MS ions at m/z 171.0998, 172.0718, 172.04081, 213.1463, 181.0722 and 151.1114, respectively. There is achieved exact coefficient of linear correlation (|r|=1) between theory and experiment of ion at m/z 172.04081. The major challenge to quantify MTZ in urine sample is that it stabilizes cations [M+H]+ of two tautomers, which equilibrium varies drastically within the standard linear calibration dynamic range. The fragmentation patterns depend on analyte tautomers and it unambiguous assignment in multicomponent samples with complex sample matrix effect (SME) is unable to be made without mediation to an independent physico-chemical law. To solve the problem, herein, is used, again, above equation, which is designed a bridge between quantitative and multidimensional structural analytical chemistry, when is used complementary with Arrhenius’s quantum chemical diffusion parameter (DQC.) There is achieved |r|=0.98 of D”SD=f(DQC’) examining tautomeric molecular and fragment ions of MTZ. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"43 1","pages":"322 - 348"},"PeriodicalIF":0.0,"publicationDate":"2022-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"83697831","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 6

Application of Response Surface Methodology for Optimization and Separation of Free Glycerol, Diglyceroids and Triglycerides from Biodiesel Using PES Ultrafiltration Membrane 响应面法在PES超滤膜优化分离生物柴油游离甘油、二甘油酯和甘油三酯中的应用

Analytical Chemistry Letters Pub Date : 2022-05-04 DOI: 10.1080/22297928.2022.2055490

P. Bansod, S. Dharaskar, Shyam M Kodape

{"title":"Application of Response Surface Methodology for Optimization and Separation of Free Glycerol, Diglyceroids and Triglycerides from Biodiesel Using PES Ultrafiltration Membrane","authors":"P. Bansod, S. Dharaskar, Shyam M Kodape","doi":"10.1080/22297928.2022.2055490","DOIUrl":"https://doi.org/10.1080/22297928.2022.2055490","url":null,"abstract":"Abstract The available natural energy sources are inadequate to satisfy the demands of an increasing population and control environmental pollution. It is critical to prioritise alternative energy sources like biodiesel. Biodiesel is an eco-sustainable and renewable energy source. But impurities present in biodiesel causes problems in internal combustion engine and emission of hazards gases after burning, it must be separated in accordance with international standards. Conventional techniques are insufficient for separating impurities from biodiesel. Membrane separation technology has been found to be a cost-effective and environmentally friendly technique for biodiesel separation. In this study, 10 KDa polyethersulfone ultrafiltration membranes were used to separate impurities from biodiesel such as free glycerol, diglyceroids, and triglycerides. The response surface was used to analyse the influence of operating variables such as temperature, transmembrane pressure and water addition on impurity separation as well as optimization. The impurities were separated according to international standards and at optimal conditions, 96.45 % free glycerol, 54.37 % diglyceroids and 61.66 % triglycerides were removed at 60°C, 0.3 wt% water addition, and 2.6 bars transmembrane pressure. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"29 1","pages":"380 - 390"},"PeriodicalIF":0.0,"publicationDate":"2022-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87522716","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 1

A Qbd Driven Approach for Development and Validation of an RP-UHPLC Method for Simultaneous Estimation of Ofloxacin and Fluconazole: An Application to Pharmaceutical Analysis Qbd驱动的RP-UHPLC同时测定氧氟沙星和氟康唑的方法的建立和验证:在药物分析中的应用

Analytical Chemistry Letters Pub Date : 2022-05-04 DOI: 10.1080/22297928.2022.2063069

S. Sanap, Amol Chhatrapati Bisen, Abhijit Deb Choudhury, S. Verma, Mukesh Kumar, R. Bhatta

{"title":"A Qbd Driven Approach for Development and Validation of an RP-UHPLC Method for Simultaneous Estimation of Ofloxacin and Fluconazole: An Application to Pharmaceutical Analysis","authors":"S. Sanap, Amol Chhatrapati Bisen, Abhijit Deb Choudhury, S. Verma, Mukesh Kumar, R. Bhatta","doi":"10.1080/22297928.2022.2063069","DOIUrl":"https://doi.org/10.1080/22297928.2022.2063069","url":null,"abstract":"Abstract A simple reverse-phase UHPLC (RP-UHPLC) analytical method was developed and validated according to International Council on Harmonization (ICH) guidelines for simultaneous estimation of ofloxacin (OFX) and fluconazole (FCZ) using a Response surface aided central composite design (CCD, Design-Expert®, Version 11.1.2.0). The method was validated for linearity, selectivity, sensitivity, accuracy, precision, limits of detection and quantification, solution stability and robustness. OFX and FCZ separation were achieved using Agilent 1290 Infinity II UHPLC system encompassed with Waters Atlantis® T3 (150 × 4.6 mm2 i.d., 3 µm particle size) column, water containing 0.1% v/v formic acid and methanol as isocratic mobile phase. OFX and FCZ eluted at 4.1 and 10.5 min with no interference of the excipients used in formulation at λmax 260 nm. The developed method was envisaged to determine total drug content, in vitro drug release study and ex-vivo corneal permeation study of conventional as well as novel drug delivery formulations. The proposed method is simple, cost-effective, dependable and reproducible and could be used for the regular analysis of OFX and FCZ in bulk and quality controls in the research and pharmaceutical industries. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"42 1","pages":"310 - 321"},"PeriodicalIF":0.0,"publicationDate":"2022-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"86886954","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 2

Enantiomeric Separation of (R)-5-(1-Hydroxyethyl)-2-(pyridine- 2-yl)-[1, 3, 4]-thiadiazole, an Intermediate of Nafithromycin on Immobilized Amylose Based Stationary Phase 固定化直链淀粉固定相分离纳霉素中间体(R)-5-(1-羟乙基)-2-(吡啶-2-基)-[1,3,4]-噻二唑对映体

Analytical Chemistry Letters Pub Date : 2022-05-04 DOI: 10.1080/22297928.2022.2073261

Rajiv A. Jadhav, V. Ahirrao, Rushikesh H. Patil, K. More, Anil R. Tile, V. Rane, Pravin S. Sonawane, R. Yeole

{"title":"Enantiomeric Separation of (R)-5-(1-Hydroxyethyl)-2-(pyridine- 2-yl)-[1, 3, 4]-thiadiazole, an Intermediate of Nafithromycin on Immobilized Amylose Based Stationary Phase","authors":"Rajiv A. Jadhav, V. Ahirrao, Rushikesh H. Patil, K. More, Anil R. Tile, V. Rane, Pravin S. Sonawane, R. Yeole","doi":"10.1080/22297928.2022.2073261","DOIUrl":"https://doi.org/10.1080/22297928.2022.2073261","url":null,"abstract":"Abstract Chiral high performance liquid chromatography method for the separation of (R)-5-(1- Hydroxyethyl)-2-(pyridine-2-yl)-[1, 3, 4]-thiadiazole (R-alcohol) an intermediate of new antibiotic Nafithromycin (NFT) has been developed and validated. NFT is a ketolide class of antibiotic currently under Phase III clinical trials in India to treat community acquired bacterial pneumonia. Chiral separation of the enantiomers with resolution >2 was accomplished on Chiralpak IA column using a mixture of n-hexane and isopropanol (IPA) in the ratio of (90:10; v/v) as an elution solvent, run at a flow rate of 1.2 mL.min-1. The column was maintained at 25°C. The analytes were detected at 254 nm. The developed method was extensively validated as per the international council for harmonisation of technical requirements for pharmaceuticals for human use guideline. Sensitivity of the method was adequate to control the passage of unwanted enantiomer to next step with limit of quantification (LOQ) of the undesired enantiomer (S)-5-(1-Hydroxyethyl)-2-(pyridine- 2-yl)-[1, 3, 4]-thiadiazole (S-alcohol) of 0.37 µgmL-1. Mean recovery of the S-alcohol was 98.9±8.7%. During development influence of column oven temperature on the chiral separation was assessed. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"95 1","pages":"409 - 418"},"PeriodicalIF":0.0,"publicationDate":"2022-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"83922032","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 1

Highly Impressive Sonophotocatalytic Degradation of Acid Red 17 using visible light induced Ag Impregnated ZnO Photocatalyst 可见光诱导银浸渍ZnO光催化剂对酸性红17的声光催化降解研究

Analytical Chemistry Letters Pub Date : 2022-05-04 DOI: 10.1080/22297928.2022.2073262

Azmat Ali Khan, Fatima Khitab, J. Shah, M. R. Jan

{"title":"Highly Impressive Sonophotocatalytic Degradation of Acid Red 17 using visible light induced Ag Impregnated ZnO Photocatalyst","authors":"Azmat Ali Khan, Fatima Khitab, J. Shah, M. R. Jan","doi":"10.1080/22297928.2022.2073262","DOIUrl":"https://doi.org/10.1080/22297928.2022.2073262","url":null,"abstract":"Abstract Dyestuffs are very persistent in nature and are present in large number in wastewater of different industries. The wastewater of different industries contains many pollutants which are hazardous for human health and environment. In the present study, sonophotocatalytic degradation of Acid red 17 (AR-17) dye in aqueous solution was investigated using silver impregnated zinc oxide (Ag/ZnO). Silver impregnated zinc oxide (Ag/ZnO) catalyst was prepared by wet impregnation method and characterized by SEM, EDX, XRD and band gap. Removal of dye was carried out at 40 kHz frequency ultrasound waves under visible light (Tungsten lamp) of 100 W. The effect of various operating conditions and reagents like H2O2 concentration, pH of the solution, amount of catalyst and concentration of AR-17 dye were investigated. At the own pH of dye using 7 mmole H2O2 concentration 92.9 % degradation of acid red 17 was observed. The degradation increased with increase in irradiation and sonication time of 30 minutes and with 0.25 g /100 mL Ag/ZnO highest degradation 92.94 % was found. The TOC analysis was also carried out sonophotocatalytically and 80 % removal of total organic compounds was observed. The degradation of AR-17 followed pseudo-second-order kinetics with high value of correlation coefficient. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"47 1","pages":"358 - 370"},"PeriodicalIF":0.0,"publicationDate":"2022-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76524889","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Rapid, Greener and One-pot Four Component Synthesis of 1, 4-Dihydropyridine Derivatives 快速、绿色、一锅四组分合成1,4 -二氢吡啶衍生物

Analytical Chemistry Letters Pub Date : 2022-04-27 DOI: 10.1080/22297928.2022.2036233

Kiranba F. Jadeja, H. Joshi

引用次数: 0

Method Validation and Measurement Uncertainty Evaluation of the Radiochemical Procedure for the Determination of 231Pa in Siliceous Cake by Gamma Spectrometry 放射化学法测定硅饼中231Pa的方法验证及测量不确定度评定

Analytical Chemistry Letters Pub Date : 2022-03-04 DOI: 10.1080/22297928.2022.2049869

A. Dalvi, P. S. Remya Devi, K. K. Swain

{"title":"Method Validation and Measurement Uncertainty Evaluation of the Radiochemical Procedure for the Determination of 231Pa in Siliceous Cake by Gamma Spectrometry","authors":"A. Dalvi, P. S. Remya Devi, K. K. Swain","doi":"10.1080/22297928.2022.2049869","DOIUrl":"https://doi.org/10.1080/22297928.2022.2049869","url":null,"abstract":"Abstract An in-house radiochemical procedure for the separation of 231Pa from siliceous cake - a waste stream of monazite processing plant, followed by its determination using gamma ray spectrometry, has been developed in our laboratory. Evaluation of reliability of analytical results of the radiochemical procedure is important for validating the fitness of purpose of an analytical method. The present paper describes the statistical evaluation of the analytical results obtained, by estimating the overall uncertainty in the measurement process. The bottom-up approach, also called as ISO approach (ISO/IEC guide 98-3:2008), was adopted to evaluate the overall uncertainty in which the individual sources were identified, evaluated and propagated. The major contribution to the combined uncertainty in measurement of 231Pa was from efficiency calibration. Besides this, counting statistics in the sample and chemical yield of the process incorporated significant contribution to combined uncertainty. The precision of the results obtained was found to be acceptable, as ascertained by the Horwitz Ratio, for the performance of a single laboratory. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"45 1","pages":"174 - 184"},"PeriodicalIF":0.0,"publicationDate":"2022-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76470982","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0