Analytical Chemistry Letters最新文献_第7页

Bioanalytical Method Development and Validation for Determination of Rifampicin and Quercetin in Rat Plasma by UHPLC-MS/MS: Applications to Pharmacokinetic Study UHPLC-MS/MS法测定大鼠血浆中利福平和槲皮素的生物分析方法的建立与验证:在药动学研究中的应用

Analytical Chemistry Letters Pub Date : 2023-01-02 DOI: 10.1080/22297928.2022.2162830

Devangkumar Tandel, K. Patel, V. Thakkar, A. Sakure, T. Gandhi

{"title":"Bioanalytical Method Development and Validation for Determination of Rifampicin and Quercetin in Rat Plasma by UHPLC-MS/MS: Applications to Pharmacokinetic Study","authors":"Devangkumar Tandel, K. Patel, V. Thakkar, A. Sakure, T. Gandhi","doi":"10.1080/22297928.2022.2162830","DOIUrl":"https://doi.org/10.1080/22297928.2022.2162830","url":null,"abstract":"Abstract UHPLC-MS/MS was utilised to quantitatively analyse Rifampicin and Quercetin-loaded Liquisolid compact in rat plasma. The UPLC Acquity C18 (1.7 μm, 2.1 × 15 mm) column and 0.5 ml/min were used to separate the analyte. In a low-pressure gradient mode, A: In water 0.1 % formic acid and B: In acetonitrile 0.1 % formic acid as the mobile phase. Sample pre-treatment was performed by protein precipitation technique with methanol and acetonitrile (1:1) from rat plasma. As an internal standard (IS), the analyte was found by tracking precursor-to-product ion transformations of 823 → 791.3 m/z for rifampicin, 303 → 257 m/z for quercetin, and 138 → 121 m/z for isoniazid in MRM mode. The proposed technique was validated for precisions (Intraday and Interday) accuracy, linearity, quantification at lower limits, and analyte recovery. The findings showed that the plasma samples inter and intra-day precision and consistency values were determined to be within the acceptable range. After orally administering Liquid solid compact and pure drug solution, which showed a substantial difference in the pace and extent of absorption, the method’s suitability for determining the pharmacokinetic profile of each drug was tested. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"21 1","pages":"60 - 72"},"PeriodicalIF":0.0,"publicationDate":"2023-01-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"82543216","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

HPTLC-Densitometric Estimation of Anti-hypertensive Drug Combination Azilsartan Medoxomil and Cilnidipine in Combined Dosage Form 降压药阿齐沙坦美多索米与西尼地平联合剂型的hptlc密度测定

Analytical Chemistry Letters Pub Date : 2023-01-02 DOI: 10.1080/22297928.2023.2195862

Dhavalsinh P. Solanki, Krunal H. Solanki, Jaineel Desai, D. Shah, U. Chhalotiya

{"title":"HPTLC-Densitometric Estimation of Anti-hypertensive Drug Combination Azilsartan Medoxomil and Cilnidipine in Combined Dosage Form","authors":"Dhavalsinh P. Solanki, Krunal H. Solanki, Jaineel Desai, D. Shah, U. Chhalotiya","doi":"10.1080/22297928.2023.2195862","DOIUrl":"https://doi.org/10.1080/22297928.2023.2195862","url":null,"abstract":"Abstract A combination of Azilsartan Medoxomil and Cilnidipine is prescribed in the treatment of Hypertension. The present work represents an accurate and precise high-performance thin layer chromatographic method for the estimation of Azilsartan Medoxomil (AZL) and Cilnidipine (CLN) in combined tablet dosage form. Pre-coated silica gel- G60 F254 aluminum sheet (100 × 100 mm, 0.2 mm layer thickness) were used as stationary phase and Ethyl Acetate: Toluene: Glacial Acetic Acid (5: 4.9: 0.1 %v/v/v) in the mixture was used as mobile phase. The method was linear in the concentration range of 200 - 2000 ng/band for AZL and 50 -500 ng/band for CLN with a correlation coefficient (r2) of 0.996 for AZL and 0.999 for CLN. The proposed method was validated with respect to linearity, accuracy, precision, and robustness as per ICH Q2 (R1) guideline. A forced degradation study was performed to assess the stability indicating the nature of the method. All the degradant peaks were well resolved from the peak of the drug without any interference. The method was successfully applied for the analysis of AZL and CLN in combined tablet formulation. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"8 1","pages":"82 - 94"},"PeriodicalIF":0.0,"publicationDate":"2023-01-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81500138","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

Enantioselective Green HPLC Method for Simultaneous Determination of Enantiomer, and Potential Impurities in Apremilast Drug Substance 对映选择性绿色高效液相色谱法同时测定阿普米司特原料药中对映体及潜在杂质

Analytical Chemistry Letters Pub Date : 2022-11-02 DOI: 10.1080/22297928.2022.2155071

C. Vijaykumar, Y. Kumar, P. Aparna, V. Marisetti

{"title":"Enantioselective Green HPLC Method for Simultaneous Determination of Enantiomer, and Potential Impurities in Apremilast Drug Substance","authors":"C. Vijaykumar, Y. Kumar, P. Aparna, V. Marisetti","doi":"10.1080/22297928.2022.2155071","DOIUrl":"https://doi.org/10.1080/22297928.2022.2155071","url":null,"abstract":"Abstract A single reversed-phase HPLC method was developed for the quantification of seven impurities of Apremilast and its enantiomer in the drug substance. An immobilized chiral stationary phase with a chiral selector “tris (3,5-dimethyl phenyl carbamate) derivative of amylose-Chiralpak IA-3 (250 mm × 4.6 mm, 3 μm) was employed to achieve the desired separation. A mobile phase consists of buffer (0.01M NH4HCO3, PH 8.0) and acetonitrile in the ratio 50:50 (v/v) and is pumped at a flow rate of 0.4 mL/min with an isocratic elution mode. The column oven temperature is set at 25°C, and the chromatographic output is monitored at 225 nm with a total run time of 45 min. A test concentration of 500 µg/mL of Apremilast in the mobile phase is used with an injection volume of 10 µL. Induced degradation studies were carried out to study the intrinsic chemical behavior of the drug. The degradation sample solutions were utilized to demonstrate the stability-indicating nature of the developed analytical method. The obtained mass number [M+H]+ for the primary degradation product formed in acid hydrolysis was identified as 418.36 and in base hydrolysis 478.12. The two impurities were identified as impurity-5(Deacetylated impurity), and impurity-2(open ring acid impurity), respectively, and the degradation pathways were established. Following ICH Q2 and USP<1225>guidelines, complete method validation was carried out. The RSD for the drug and impurities in interday and intraday studies are less than 4.0%, and the recoveries for the impurities are between 96.1-102.1% and linearity r ≥ 0.9997. LOQ results for the drug and impurities are between 0.052 µg/mL and 0.107 µg/mL, and LOD results are between 0.016 µg/mL and 0.032 µg/mL. The greenness of the method was evaluated by using an analytical eco scale, GAPI, and AGREE, and it was found that the method is green. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"30 1","pages":"691 - 714"},"PeriodicalIF":0.0,"publicationDate":"2022-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"75316774","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

Execution of Quality by Design Approach for Preparation and Optimization of Inclusion Complexes: In-vivo and ex-vivo Assessment 包合物制备和优化的质量设计方法:体内和体外评价

Analytical Chemistry Letters Pub Date : 2022-11-02 DOI: 10.1080/22297928.2022.2159521

Neha Bajwa, P. Singh, Srishti Naryal, Trisha Sharma, Puran Singh Sijwal, Ashish Baldi

{"title":"Execution of Quality by Design Approach for Preparation and Optimization of Inclusion Complexes: In-vivo and ex-vivo Assessment","authors":"Neha Bajwa, P. Singh, Srishti Naryal, Trisha Sharma, Puran Singh Sijwal, Ashish Baldi","doi":"10.1080/22297928.2022.2159521","DOIUrl":"https://doi.org/10.1080/22297928.2022.2159521","url":null,"abstract":"Abstract The inclusion complex of α, β-arteether with β-cyclodextrin was prepared. The ratio was selected by implementing the QbD approach to get the best host-guest complex ratio. Further, the formation of the best complex was compared with stability analysis. Also, the enhancement in dissolution profile, as well as solubility, was compared with the pure α, β-arteether. The cyclodextrin derivative with maximum enhanced solubility and best dissolution profile was further used for PKPD modeling, permeability studies, and in-vivo and ex-vivo studies. By QbD approach as well as phase solubility studies it was confirmed that 1:1 fits best for the ART-CD inclusion complex formation. This was substantiated by a saturation solubility investigation, which found that in the presence of PVPK30, the solubility of α, β-arteether was enhanced by 77.05 times. The crystalline nature of the drug was lost or diminished greatly in the inclusion complex, showing the drug was present in a solubilized form in the formulation, according to scanning electron microscopy, X-ray diffraction, and differential scanning calorimetry. Further, the complex powder was converted into spheroids by the spheronization technique and filled in empty enteric-coated shells. In vitro release studies for spheroids-filled enteric capsules were carried out for 6 h by progressive dissolution technique. The pharmacokinetic model using Ecosim Pro 6.2.0 software confirms the enhancement of the bioavailability of the arteether. Further, the in vivo studies also confirm the enhancement in absolute bioavailability by 48.29% when compared with i.v. data of pure drugs. The complex shows an 11% maximum enhancement in antimalarial activity when compared with pure drugs. From the research, it was concluded that inclusion complexation is a suitable approach to improvise the solubility as well as bioavailability of hydrophobic drugs like α, β-arteether. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"26 1","pages":"715 - 729"},"PeriodicalIF":0.0,"publicationDate":"2022-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"86105409","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

Repurposing of Existing Pharmaceutical Drugs Against Monkey-pox Virus: An In Silico Study 现有抗猴痘病毒药物的再利用:一项计算机研究

Analytical Chemistry Letters Pub Date : 2022-11-02 DOI: 10.1080/22297928.2022.2157224

K. Sarkar, R. Das

{"title":"Repurposing of Existing Pharmaceutical Drugs Against Monkey-pox Virus: An In Silico Study","authors":"K. Sarkar, R. Das","doi":"10.1080/22297928.2022.2157224","DOIUrl":"https://doi.org/10.1080/22297928.2022.2157224","url":null,"abstract":"Abstract Monkeypox virus (MPXV) is considered as zoonotic disease with characteristics comparable to smallpox virus. The disease is now a global epidemic concern. Currently, tecovirimat is approved by US Food and Drug Administration (FDA) for MPXV treatment. The aim of this in silico study is to repurpose approved pharmaceutical drugs as potential inhibitors of MPXV target. In this study, molecular docking was performed on 406 pharmaceutical drugs, and results were compared with reference tecovirimat. Results showed that 7 compounds, bictegravir, glimepiride, glyburide, lasmiditan, olaparib, rimegepant, and ubrogepant, have shown higher binding energies compared to the reference. After that, these best hits were further assessed by 100 ns molecular dynamics simulation and the best results were observed for bictegravir, glimepiride, glyburide, olaparib, and ubrogepant. The docking analysis was further validated by molecular mechanics Poisson-Boltzmann surface area (MM-PBSA) binding free energy calculations. In addition, pharmacokinetics and density functional theory (DFT) studies were also discussed for these best hits. In conclusion, three compounds, bictegravir, glimepiride, and glyburide, have satisfied all the criteria for better leads against MPXV. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"81 1","pages":"655 - 670"},"PeriodicalIF":0.0,"publicationDate":"2022-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"85137016","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

Green Chemistry Method Based on Native Fluorescence for Estimation of Recently Approved Anti-neoplastic Drug Sotorasib 基于天然荧光的绿色化学方法评价新批准的抗肿瘤药物Sotorasib

Analytical Chemistry Letters Pub Date : 2022-11-02 DOI: 10.1080/22297928.2022.2160273

H. Salem, Noha Abdal-Karim, Bahaa Omran, Abdel-Rahman Abdel-Gayed, Mazen Atef, Shrouq Bahaa, M. Abdelgaleel

引用次数: 0

Phytochemical Constituents and Bioactivity Profiles of Citrus Genus from India 印度柑橘属植物化学成分及生物活性研究

Analytical Chemistry Letters Pub Date : 2022-11-02 DOI: 10.1080/22297928.2022.2157223

Rony Bhowal, Sony Kumari, C. Sarma, P. Suprasanna, Puja Roy

引用次数: 2

Hot Melt Extrusion Assisted Felodipine Loaded Liquid Crystal Precursor with Enhanced Solubility and Sustained Drug Release Characteristics 热熔挤压辅助非洛地平负载液晶前体增强溶解度和缓释特性

Analytical Chemistry Letters Pub Date : 2022-11-02 DOI: 10.1080/22297928.2022.2159523

Sushank Suryawanshi, R. Pawar, R. Gonnade, Sharvil Patil

{"title":"Hot Melt Extrusion Assisted Felodipine Loaded Liquid Crystal Precursor with Enhanced Solubility and Sustained Drug Release Characteristics","authors":"Sushank Suryawanshi, R. Pawar, R. Gonnade, Sharvil Patil","doi":"10.1080/22297928.2022.2159523","DOIUrl":"https://doi.org/10.1080/22297928.2022.2159523","url":null,"abstract":"Abstract Glyceryl monooleate (GMO) forms cubic mesophase upon hydration with sustained drug release characteristics. However its stickiness and stiffness often creates processing challenges for preparation of formulations. Felodipine (FLD), BCS class II molecule was used as model drug. Thus objective of the current work was to increase manufacturing feasibility of GMO using polymer and to enhance the release of felodipine by preparing LC precursors using HME. HPMC E5 polymer was selected for processing of FLD. Batch optimization was done using 23 Factorial design. The prepared batches were characterized for DSC, FTIR, hot stage microscopy (HSM), plane polarized light microscopy (PPL), PXRD and in vitro dissolution studies. The processing of FLD using HME process showed amorphization as revealed by PXRD studies. DSC and HSM studies showed solubilization of FLD in the molten mass of GMO and HPMC E5 confirming formation of solid dispersion. PPL demonstrated formation of cubic LC phase by GMO upon hydration of prepared formulations. The optimized batch of felodipine showed significant improvement in the dissolution profile of FLD with extended release profile. HME assisted liquid crystal precursors could act as promising formulations for BCS II drugs requiring extended drug release profile with improved processing feasibility of GMO. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"86 1","pages":"745 - 760"},"PeriodicalIF":0.0,"publicationDate":"2022-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"89866523","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

Biophysical, Calorimetric, Zeta Potential, Voltammetric and Computational Insights into the Interaction of An Antimuta-genic Agent with Human Serum Albumin 生物物理，量热，Zeta电位，伏安和计算洞察抗诱变剂与人血清白蛋白的相互作用

Analytical Chemistry Letters Pub Date : 2022-11-02 DOI: 10.1080/22297928.2022.2151375

Roopa S. Naik, J. Seetharamappa

引用次数: 0

Characterization of Degradation Products of Lifitegrast by Mass Spectrometry: Development and Validation of a Stability-indicating Reversed Phase HPLC Method lifitgrast降解产物的质谱表征:稳定性指示反相高效液相色谱法的建立和验证

Analytical Chemistry Letters Pub Date : 2022-11-02 DOI: 10.1080/22297928.2022.2159522

Ajay Kumar, R. Chalannavar

{"title":"Characterization of Degradation Products of Lifitegrast by Mass Spectrometry: Development and Validation of a Stability-indicating Reversed Phase HPLC Method","authors":"Ajay Kumar, R. Chalannavar","doi":"10.1080/22297928.2022.2159522","DOIUrl":"https://doi.org/10.1080/22297928.2022.2159522","url":null,"abstract":"Abstract Lifitegrast API was subjected to forced degradation studies under various conditions of hydrolysis (acidic, alkaline, and neutral/water), oxidation, photolysis, and thermal as prescribed by International Conference on Harmonisation guideline Q1A (R2). A short and simple reversed phase HPLC method was developed. The method was developed on a Shimadzu Ultra C18, (100 x 2.1) mm, 3.0 μm column. The gradient method consisted of 0.1% orthophosphoric acid as mobile phase A and mixture of acetonitrile and methanol in the ratio of 50:50 (v/v) as mobile phase B. The flow rate of the mobile phase was 0.8 mL/min. The developed method was validated using ICH Q2 (R1) guidelines. The parameters considered for method validation were solution stability, specificity, DL/QL, linearity, accuracy, precision and robustness. The drug showed significant degradation in acidic and alkaline conditions while slight degradation was observed in oxidative condition. The drug was found stable in water, photolytic and thermal conditions. The characterization of three major degradation products (DP1, DP2, and DP3) was done with LC-Q-TOF-MS/MS in combination with accurate mass measurements. The most probable mechanisms for the formation of DPs have been proposed on the basis fragmentation pattern. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"14 1","pages":"730 - 744"},"PeriodicalIF":0.0,"publicationDate":"2022-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"88087436","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