Journal of Pharmaceutical and Biomedical Analysis Open最新文献

Miniaturized sample preparation strategies for the determination of N-nitrosamines in pharmaceutical products: A comprehensive review 药品中n -亚硝胺的小型化样品制备方法综述

Journal of Pharmaceutical and Biomedical Analysis Open Pub Date : 2025-07-22 DOI: 10.1016/j.jpbao.2025.100081

Almir Custodio Batista Junior, Yuri Arrates Rocha, Andrea Rodrigues Chaves

{"title":"Miniaturized sample preparation strategies for the determination of N-nitrosamines in pharmaceutical products: A comprehensive review","authors":"Almir Custodio Batista Junior, Yuri Arrates Rocha, Andrea Rodrigues Chaves","doi":"10.1016/j.jpbao.2025.100081","DOIUrl":"10.1016/j.jpbao.2025.100081","url":null,"abstract":"<div><div>N-Nitrosamines (NAs) are classified as potent mutagenic impurities, raising substantial concerns due to their presence in various consumer products, including pharmaceuticals products. The detection of NAs in valsartan-containing medicines in 2018 led regulatory agencies to establish strict guidelines for permissible levels in drug formulations. The standard-gold analytical techniques for NAs determination have been chromatographic techniques (liquid and gas chromatography) coupled with mass spectrometry system, which present higher sensibility and accuracy for target NAs. However, accurate determination of NAs in medicines remains challenging due to their trace-level concentrations and susceptibility to matrix effects, carryover, and contamination of the analytical instrumentation, emphasizing the need for robust sample preparation strategies. Traditional sample preparation methods, although effective, often involve high consumption of solvents, samples, and extraction phases, along with substantial waste generation. In response, miniaturized sample preparation techniques have emerged as sustainable alternatives, offering reduced solvent usage, minimal sample requirements, and lower energy consumption, all while maintaining analytical performance. These green approaches not only align with sustainable analytical practices but also enhance efficiency and environmental compliance in pharmaceutical analysis. This review provides a comprehensive overview of recent advancements in miniaturized sample preparation strategies for the determination of NAs in pharmaceutical products, highlighting their analytical merits and potential for regulatory adoption.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"6 ","pages":"Article 100081"},"PeriodicalIF":0.0,"publicationDate":"2025-07-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144704536","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

A green and robust LC–MS/MS bioanalytical method for sulopenem etzadroxil and probenecid: Optimization, validation, and pharmacokinetic application 绿色高效液相色谱-质谱/质谱联用分析苏罗培南依扎罗西和丙苯酸的方法：优化、验证及药动学应用

Journal of Pharmaceutical and Biomedical Analysis Open Pub Date : 2025-07-22 DOI: 10.1016/j.jpbao.2025.100083

Niloufer Tasnim Khazi, Kumaraswamy Gandla, Lalitha Repudi

{"title":"A green and robust LC–MS/MS bioanalytical method for sulopenem etzadroxil and probenecid: Optimization, validation, and pharmacokinetic application","authors":"Niloufer Tasnim Khazi, Kumaraswamy Gandla, Lalitha Repudi","doi":"10.1016/j.jpbao.2025.100083","DOIUrl":"10.1016/j.jpbao.2025.100083","url":null,"abstract":"<div><div>A novel, green, and robust Liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was developed and validated for the simultaneous quantification of sulopenem etzadroxil and probenecid in rat plasma, with application to pharmacokinetic studies. Method development was guided by a Box–Behnken Design and response surface methodology, optimizing key chromatographic variables—ethanol proportion (40–60 %), flow rate (0.8–1.2 mL/min), and mobile phase pH (2.8–3.2)—to achieve maximum resolution, peak area, and analytical reproducibility. Chromatographic separation was performed on a Kromasil C18 column using ethanol and 0.1 % TFA (50:50, v/v) as the mobile phase. Mass spectrometric detection employed selected reaction monitoring in positive ion mode using an LC-MS/MS instrument. The method exhibited excellent linearity (10–400 ng/mL), low limits of detection (LOD: ∼3 ng/mL), and quantification (LOQ: ∼9 ng/mL) for both analytes, with recovery rates > 93 % and %CVs < 15 %. Greenness and sustainability assessments using analytical GREEnness metric (AGREE), analytical GREEnness metric for sample PREParation (AGREEprep), complementary green analytical procedure index (ComplexGAPI), Eco-Scale, and Blue applicability grade index (BAGI) confirmed the method’s environmental compatibility and analytical reliability, with scores exceeding 65 across all tools. This validated method demonstrates high sensitivity, reproducibility, and environmental responsibility, rendering it suitable for routine bioanalytical and pharmacokinetic applications.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"6 ","pages":"Article 100083"},"PeriodicalIF":0.0,"publicationDate":"2025-07-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144695367","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

N-nitrosamine risk assessment in pharmaceuticals: Where are we from a regulatory point of view in 2025? 药品中n -亚硝胺风险评估：从监管的角度来看，2025年我们在哪里？

Journal of Pharmaceutical and Biomedical Analysis Open Pub Date : 2025-07-21 DOI: 10.1016/j.jpbao.2025.100084

Yue Zhang, Joëlle Widart, Eric Ziemons, Philippe Hubert, Cédric Hubert

{"title":"N-nitrosamine risk assessment in pharmaceuticals: Where are we from a regulatory point of view in 2025?","authors":"Yue Zhang, Joëlle Widart, Eric Ziemons, Philippe Hubert, Cédric Hubert","doi":"10.1016/j.jpbao.2025.100084","DOIUrl":"10.1016/j.jpbao.2025.100084","url":null,"abstract":"<div><div><em>N</em>-nitrosamines have been a concern for decades due to their potential mutagenicity and widespread occurrence across various matrices. While evidence suggests carcinogenicity in animals, their potential carcinogenicity in humans has prompted their initial inclusion in the “cohort of concern” since in ICH M7(R1), and the current ICH M7(R2) guideline is now in effect. Intensified control of <em>N</em>-nitrosamines began in 2018 following the detection of <em>N</em>-nitrosodimethylamine in valsartan-containing products. Subsequent investigations revealed <em>N</em>-nitrosamine contamination across multiple drug classes, triggering widespread recalls, withdrawals, and regulatory actions. Recently, the emergence of <em>N</em>-nitrosamine drug substance-related impurities and drug linker-related impurities has drawn additional regulatory attention. This review presents the methodologies used to determine the acceptable daily intake of <em>N</em>-nitrosamines and traces the evolution of regulatory guidelines, offering a comparative analysis of the 3-step investigation approaches adopted by the European Medicines Agency and Food and Drug Administration. It provides a comprehensive examination of potential root causes for <em>N</em>-nitrosamine contamination, outlines the analytical requirements for confirmatory testing, as well as mitigation strategies to prevent or minimize contamination. Additionally, the review summarizes risk assessment tools used to predict <em>N</em>-nitrosamine formation. By presenting a comprehensive workflow for impurity investigations, this review aims to assist industrial stakeholders in managing <em>N</em>-nitrosamine risks, ensuring regulatory compliance, and safeguarding public health.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"6 ","pages":"Article 100084"},"PeriodicalIF":0.0,"publicationDate":"2025-07-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144695369","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

Comparative analysis of MS/MS search algorithms in label-free shotgun proteomics for monitoring host-cell proteins using trapped ion mobility and ddaPASEF 利用捕获离子迁移率和ddaPASEF监测宿主细胞蛋白的无标记鸟枪蛋白组学中MS/MS搜索算法的比较分析

Journal of Pharmaceutical and Biomedical Analysis Open Pub Date : 2025-07-21 DOI: 10.1016/j.jpbao.2025.100082

Somar Khalil, Michel Plisnier

{"title":"Comparative analysis of MS/MS search algorithms in label-free shotgun proteomics for monitoring host-cell proteins using trapped ion mobility and ddaPASEF","authors":"Somar Khalil, Michel Plisnier","doi":"10.1016/j.jpbao.2025.100082","DOIUrl":"10.1016/j.jpbao.2025.100082","url":null,"abstract":"<div><div>Host cell proteins (HCPs) are critical quality attributes that can impact the safety, efficacy, and quality of biotherapeutics. Label-free shotgun proteomics is a vital approach for HCP monitoring, yet the choice of tandem mass spectrometry (MS/MS) search algorithms directly influences identification depth and quantification reliability. In this study, six prominent MS/MS search tools (Mascot, MaxQuant, SpectroMine, FragPipe, Byos, and PEAKS) were systematically benchmarked for their performance on complex samples spiked with isotopically labeled proteins from Chinese hamster ovary cells. The data were acquired using trapped ion mobility spectrometry and parallel accumulation–serial fragmentation in data-dependent acquisition mode. Key performance metrics, including peptide and protein identifications, data extraction precision, fold-change (FC) accuracy, linearity, and measurement trueness, were evaluated. A Bayesian modeling framework with Hamiltonian Monte Carlo sampling was employed to robustly estimate FC means and variances, alongside local false discovery rates through posterior probability calibration. Bayesian decision theory, implemented via expected utility maximization, was used to balance accuracy against posterior uncertainty and provide a probabilistic assessment of each tool’s performance. Through this cumulative analysis, variability across tools was observed: Byos and SpectroMine excelled in quantitative accuracy with minimal bias, FragPipe provided high precision and quantifiability, PEAKS offered deep protein coverage, Mascot showed strong trueness, and MaxQuant exhibited moderate identification performance with greater variability at lower spike levels. This study establishes a rigorous, data-driven framework for tool benchmarking and offers guidance for selecting MS/MS tools suited to HCP monitoring in biopharmaceutical development.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"6 ","pages":"Article 100082"},"PeriodicalIF":0.0,"publicationDate":"2025-07-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144695366","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

Design of experiments-assisted UPLC method for quantification of nitrosamine impurities in glimepiride and lobeglitazone sulfate: A green chemistry approach 格列美脲和硫酸洛贝列酮亚硝胺杂质定量的实验辅助超高效液相色谱法设计：绿色化学方法

Journal of Pharmaceutical and Biomedical Analysis Open Pub Date : 2025-05-05 DOI: 10.1016/j.jpbao.2025.100078

KiranKumar Chagarlamudi , Venkata Kanaka Srivani Maddala , Kumaraswamy Gandla

{"title":"Design of experiments-assisted UPLC method for quantification of nitrosamine impurities in glimepiride and lobeglitazone sulfate: A green chemistry approach","authors":"KiranKumar Chagarlamudi , Venkata Kanaka Srivani Maddala , Kumaraswamy Gandla","doi":"10.1016/j.jpbao.2025.100078","DOIUrl":"10.1016/j.jpbao.2025.100078","url":null,"abstract":"<div><div>A robust ultra-performance liquid chromatography (UPLC) method was developed and systematically optimized using a Design of Experiments (DoE) approach for the simultaneous quantification of glimepiride, lobeglitazone sulfate, nitrosamine impurity-3 (IMP-3), and impurity-1 (IMP-1) in the marketed LOBG-G1 formulation. Critical method parameters, including organic phase composition, flow rate, and mobile phase pH, were identified through a comprehensive risk assessment and subsequently optimized using a Box-Behnken design. The final chromatographic conditions—50 % organic phase composition, a flow rate of 0.2 mL/min, and a mobile phase pH of 2.6—ensured efficient separation and quantification of all four analytes. The method was validated in accordance with ICH guidelines, demonstrating excellent linearity (r² > 0.999), high accuracy, and precision, with low relative standard deviation values. Stability studies conducted under different stress conditions revealed significant degradation of all four compounds in acidic, alkaline, and oxidative environments. Degradation products were further characterized using LC-MS/MS analysis, confirming their structural identity. In addition to its analytical performance, the method's environmental sustainability was evaluated using multiple green analytical chemistry assessment tools. The DoE-guided UPLC method offers a highly sensitive, selective, and reproducible analytical platform for the detection of nitrosamine impurities in antidiabetic drugs, providing enhanced method understanding while aligning with sustainability principles.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"5 ","pages":"Article 100078"},"PeriodicalIF":0.0,"publicationDate":"2025-05-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143907640","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

Advancing biomedical analysis: Harnessing laser-induced graphene for next-gen of low-cost sensor technology 推进生物医学分析：利用激光诱导石墨烯用于下一代低成本传感器技术

Journal of Pharmaceutical and Biomedical Analysis Open Pub Date : 2025-04-26 DOI: 10.1016/j.jpbao.2025.100077

Elsa Maria Materón , Liana Melo Lins de Azevedo , Juliana Martins Dias , Ketley Caroline Rocha Pereira , Gustavo Miguel Sousa , Matheus Santos Dias , Camila Marchetti Maroneze , Daiane Dias , Cecilia de Carvalho Castro Silva

{"title":"Advancing biomedical analysis: Harnessing laser-induced graphene for next-gen of low-cost sensor technology","authors":"Elsa Maria Materón , Liana Melo Lins de Azevedo , Juliana Martins Dias , Ketley Caroline Rocha Pereira , Gustavo Miguel Sousa , Matheus Santos Dias , Camila Marchetti Maroneze , Daiane Dias , Cecilia de Carvalho Castro Silva","doi":"10.1016/j.jpbao.2025.100077","DOIUrl":"10.1016/j.jpbao.2025.100077","url":null,"abstract":"<div><div>As biosensors and biomedical devices gain increasing importance in everyday diagnostics and health status monitoring, the need to develop and improve their reliability and versatility becomes more pronounced. In this context, the search for new materials for biosensors and biomedical devices has intensified, leading to the emergence of laser-induced graphene (LIG) as a promising candidate. LIG's environmentally sustainable nature, cost-effectiveness, and significant potential for large-scale graphene production and directed writing electronics circuits make it very interesting. In this review, we provide an overview of the mechanisms and precursor materials involved in LIG production, strategies to enhance graphene properties through the <em>in-situ</em> generation of hybrid materials via direct laser writing, and the crucial role of LIG in the development of cost-effective, point-of-care, and wearable devices for medical diagnosis and real-time health status monitoring.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"5 ","pages":"Article 100077"},"PeriodicalIF":0.0,"publicationDate":"2025-04-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143882125","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

Determination of rapid and sensitive extraction of colchicine from Colchicum baytopiorum and Colchicum decaisnei leaves by HPLC-UV method 高效液相色谱-紫外分光光度法测定秋水仙叶和秋水仙叶中秋水仙碱的快速灵敏提取

Journal of Pharmaceutical and Biomedical Analysis Open Pub Date : 2025-04-22 DOI: 10.1016/j.jpbao.2025.100076

Efe Deniz , Ümit Babacan , Ceren Selim , Mehmet Fatih Cengiz

{"title":"Determination of rapid and sensitive extraction of colchicine from Colchicum baytopiorum and Colchicum decaisnei leaves by HPLC-UV method","authors":"Efe Deniz , Ümit Babacan , Ceren Selim , Mehmet Fatih Cengiz","doi":"10.1016/j.jpbao.2025.100076","DOIUrl":"10.1016/j.jpbao.2025.100076","url":null,"abstract":"<div><div>This study focuses on the extraction and analysis of colchicine, a bioactive alkaloid, from the leaves of two endemic species, <em>Colchicum baytopiorum</em> (n = 13) and <em>Colchicum decaisnei</em> (n = 11), collected from Antalya, Türkiye. Colchicine, known for its pharmacological applications for the treatment of gout and cancer, was extracted using ultrasonic-assisted extraction, a more environmentally friendly alternative to conventional methods like Soxhlet and solid-liquid extraction. High-performance liquid chromatography was used for the quantification of colchicine levels in the plant samples. The method was validated in terms of linear dynamic range, limit of detection (LOD), limit of quantification (LOQ) and relative standard deviation (RSD). Results showed that LOD, LOQ and RSD values were determined to be 0.210 ppm, 0.799 ppm and 1.420, respectively. <em>C. baytopiorum</em> had a higher colchicine content (206.24 ± 87.48 ppm) compared to <em>C. decaisnei</em> (11.23 ± 23.04 ppm). These findings are consistent with previous studies, which report varying colchicine concentrations across different Colchicum species. The study suggests that genetic research could help identify the specific genes responsible for colchicine production, which could enhance its availability in pharmaceutical applications. This research contributes to understanding colchicine extraction and its potential for medical use.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"5 ","pages":"Article 100076"},"PeriodicalIF":0.0,"publicationDate":"2025-04-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143870439","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

Magnetic solid-phase extraction of Sudan dyes from beverages-coated magnetite/silica materials 饮料包覆磁铁矿/二氧化硅材料中苏丹红染料的磁固相萃取

Journal of Pharmaceutical and Biomedical Analysis Open Pub Date : 2025-03-12 DOI: 10.1016/j.jpbao.2025.100073

Yugao Guo , Xiaoxiao Niu , Boyu Li , Pei Liu , Youqing Sun , Sumin Lu

{"title":"Magnetic solid-phase extraction of Sudan dyes from beverages-coated magnetite/silica materials","authors":"Yugao Guo , Xiaoxiao Niu , Boyu Li , Pei Liu , Youqing Sun , Sumin Lu","doi":"10.1016/j.jpbao.2025.100073","DOIUrl":"10.1016/j.jpbao.2025.100073","url":null,"abstract":"<div><div>In this study, a polydopamine-coated magnetite/silica composite material (Fe<sub>3</sub>O<sub>4</sub>@SiO<sub>2</sub>/PDA) was successfully synthesized and characterized using Fourier-transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). By integrating EM-MSPE with high-performance liquid chromatography (HPLC), a novel EM-MSPE-HPLC method was established for the sensitive and accurate determination of Sudan I-IV dyes. Key experimental parameters, such as adsorbent dosage, pH, inorganic salt concentration, adsorption time, voltage, eluent type, eluent volume, and desorption time, were systematically investigated and optimized. Under optimal conditions, the method demonstrated excellent linearity (R² > 0.999) within a concentration range of 5–1000 μg L⁻¹, with limits of detection (LODs) ranging from 0.11 to 0.17 μg L⁻¹. The recoveries of Sudan dyes in real samples ranged from 89.1 % to 101.9 %, with relative standard deviations (RSDs) between 0.3 % and 3.6 %. Furthermore, the Fe<sub>3</sub>O<sub>4</sub>@SiO<sub>2</sub>/PDA adsorbent exhibited consistent performance over ten consecutive extraction cycles without significant loss in recovery efficiency. These findings demonstrate that the proposed method is accurate, reliable, and reproducible for the simultaneous determination of Sudan dyes in complex beverage matrices, offering a robust analytical approach for food safety applications.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"5 ","pages":"Article 100073"},"PeriodicalIF":0.0,"publicationDate":"2025-03-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143686909","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Direct sample introduction in high-performance liquid chromatography analysis of oily medicinal cannabis samples using surfactant-free microemulsion 使用无表面活性剂微乳液对含油药用大麻样品进行高效液相色谱分析，直接进样

Journal of Pharmaceutical and Biomedical Analysis Open Pub Date : 2025-03-11 DOI: 10.1016/j.jpbao.2025.100075

Ana Paula Lamounier, Bárbara da Conceição Coelho Cotta Cardoso, Alessandra Licursi Maia Cerqueira da Cunha

{"title":"Direct sample introduction in high-performance liquid chromatography analysis of oily medicinal cannabis samples using surfactant-free microemulsion","authors":"Ana Paula Lamounier, Bárbara da Conceição Coelho Cotta Cardoso, Alessandra Licursi Maia Cerqueira da Cunha","doi":"10.1016/j.jpbao.2025.100075","DOIUrl":"10.1016/j.jpbao.2025.100075","url":null,"abstract":"<div><div>The therapeutic use of medicinal Cannabis has raised challenges in quality control and cannabinoid quantification in oil extracts, primarily due to incompatibility with liquid chromatography systems. Surfactant-free microemulsion (SFME) systems offer a promising, efficient, and sustainable solution, enabling direct analysis by high-performance liquid chromatography. These microemulsions are dispersions of two immiscible liquids, typically oil and water, made compatible by an amphiphilic substance that interacts with both polar and nonpolar fractions. After SFME testing and critical analysis of the results, clear and homogeneous microemulsions were observed regardless of the oil-to-water ratio studied, provided that sufficient quantities of 1-octanol:1-propanol (3:10 v/v) were added. Based on the established robust working range, the 1:2 (oil:ultrapure water) ratio (% w/w) was chosen as the compromise condition, minimizing medicinal oil use while ensuring compatibility with the chromatographic system. Univariate optimization of chromatographic conditions enabled simultaneous analysis of five cannabinoids, including cannabidiol (CBD), cannabidiolic acid (CBDA), tetrahydrocannabutol (THCB), cannabinol (CBN), and tetrahydrocannabinol (Δ9-THC) using a ZORBAX Eclipse Plus C18 column at 35 °C. The method employed isocratic elution with a mobile phase of 82:18 %v/v methanol:ultrapure water containing 0.15 ± 0.05 % v/v formic acid, a 1.0 mL min<sup>−1</sup> flow rate, and a 20 μL injection volume, using the fluorescence and UV absorption detectors. This proposal offers sensitivity (LOD in the ng mL<sup>−1</sup>), selectivity, and separation efficiency, associated with low cost, minimal waste generation, and low energy demand, aligning with Green Chemistry principles.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"5 ","pages":"Article 100075"},"PeriodicalIF":0.0,"publicationDate":"2025-03-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143644376","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Interstitial fluid-based optical biosensors 基于间隙流体的光学生物传感器

Journal of Pharmaceutical and Biomedical Analysis Open Pub Date : 2025-03-10 DOI: 10.1016/j.jpbao.2025.100074

Atefeh Rahimzadeh , Abrisham Arjomandkhah , Mohammad Ali Kiani, Hamed Golmohammadi

引用次数: 0