Pub Date : 2025-02-03DOI: 10.1016/j.jpbao.2025.100061
Ensar Piskin , Fatih Ahmet Korkut , Ahmet Cetinkaya , Sibel A. Ozkan
Atorvastatin (ATR) is one of the statins that are widely used all around the world. This study presents a molecularly imprinted polymer (MIP) based electrochemical sensor for the sensitive and selective detection of ATR in binary mixtures and commercial serum samples. The designed sensor was fabricated using a photopolymerization (PP) approach on a glassy carbon electrode (GCE) using ATR as the template and acrylamide (ACR) as the functional monomer. The developed ATR/ACR@MIP-GCE sensor was evaluated electrochemically and morphologically using electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), and scanning electron microscopy (SEM). The indirect measuring method was used with a 5.0 mM [Fe(CN)6]3–/4– solution to determine the ATR in the linear range of 1.0–10.0 pM. Moreover, the sensor demonstrated excellent linearity and extremely sensitive quantification (LOQ) limit of detection (LOD) values in both biological media and standard solutions. It also performed well in terms of specificity by effectively differentiating ATR from compounds with similar structures. Excellent repeatability and reproducibility results have confirmed the reliability of the sensor. The selectivity of the ATR/ACR@MIP-GCE sensor for ATR was proven by interference studies on ezetimibe and their binary mixtures.
阿托伐他汀（ATR）是世界上广泛使用的他汀类药物之一。本研究提出了一种基于分子印迹聚合物（MIP）的电化学传感器，用于灵敏和选择性地检测二元混合物和商业血清样品中的ATR。设计的传感器以ATR为模板，丙烯酰胺（ACR）为功能单体，采用光聚合（PP）方法在玻璃碳电极（GCE）上制备。利用电化学阻抗谱（EIS）、循环伏安法（CV）和扫描电镜（SEM）对研制的ATR/ACR@MIP-GCE传感器进行了电化学和形态学评价。间接测量法采用5.0 mM [Fe(CN)6]3 - /4 -溶液，在1.0 ~ 10.0 pM线性范围内测定ATR。此外，该传感器在生物培养基和标准溶液中均表现出良好的线性和极灵敏的定量（LOQ）检测限（LOD）值。它还表现出良好的特异性，可以有效地将ATR与具有相似结构的化合物区分开来。优异的重复性和再现性结果证实了该传感器的可靠性。通过对依折替米贝及其二元混合物的干扰研究，证明了ATR/ACR@MIP-GCE传感器对ATR的选择性。
{"title":"Highly selective and sensitive detection of atorvastatin from using a MIP-based electrochemical sensor","authors":"Ensar Piskin , Fatih Ahmet Korkut , Ahmet Cetinkaya , Sibel A. Ozkan","doi":"10.1016/j.jpbao.2025.100061","DOIUrl":"10.1016/j.jpbao.2025.100061","url":null,"abstract":"<div><div>Atorvastatin (ATR) is one of the statins that are widely used all around the world. This study presents a molecularly imprinted polymer (MIP) based electrochemical sensor for the sensitive and selective detection of ATR in binary mixtures and commercial serum samples. The designed sensor was fabricated using a photopolymerization (PP) approach on a glassy carbon electrode (GCE) using ATR as the template and acrylamide (ACR) as the functional monomer. The developed ATR/ACR@MIP-GCE sensor was evaluated electrochemically and morphologically using electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), and scanning electron microscopy (SEM). The indirect measuring method was used with a 5.0 mM [Fe(CN)<sub>6</sub>]<sup>3–/4–</sup> solution to determine the ATR in the linear range of 1.0–10.0 pM. Moreover, the sensor demonstrated excellent linearity and extremely sensitive quantification (LOQ) limit of detection (LOD) values in both biological media and standard solutions. It also performed well in terms of specificity by effectively differentiating ATR from compounds with similar structures. Excellent repeatability and reproducibility results have confirmed the reliability of the sensor. The selectivity of the ATR/ACR@MIP-GCE sensor for ATR was proven by interference studies on ezetimibe and their binary mixtures.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"5 ","pages":"Article 100061"},"PeriodicalIF":0.0,"publicationDate":"2025-02-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143143655","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}
Pub Date : 2025-02-01DOI: 10.1016/j.jpbao.2025.100058
Moazaz Rashad Saed , Thikra Hasan Mathkor
Acute kidney injury (AKI) is a prevalent complication following cardiac surgery, affecting both short- and long-term survival rates. Proteinuria serves as an indicator of structural kidney damage and is increasingly recognized as a crucial marker for kidney disease and a risk factor for AKI. Free light chains (FLCs) are being investigated as potential markers for assessing the risk of kidney damage. This study aimed to validate the early detection of AKI by examining FLCs (kappa, lambda, and the kappa/lambda ratio) in serum and saliva samples. Clinical data were collected from 149 patients who underwent cardiac surgery in Baghdad, with 90 providing both saliva and serum samples for FLC evaluation. Patients were categorized based on the severity of proteinuria. Results showed that serum kappa levels were significantly elevated in patients with severe proteinuria compared to those with mild or no proteinuria. Conversely, salivary kappa levels were higher in patients with mild proteinuria than in those with severe or no proteinuria, while salivary lambda levels decreased as proteinuria severity increased. The rise in serum kappa may be attributed to immune system activation and kidney impairment. Both serum and salivary kappa demonstrated strong predictive capabilities for post-surgery AKI prognosis, outperforming lambda and the kappa/lambda ratio based on ROC analysis. The findings suggest that FLCs, particularly kappa, could be valuable in the early detection of AKI following cardiac surgery, highlighting their potential to enhance patient outcomes through proactive monitoring and intervention.
{"title":"Assessment of the serum and salivary free light chain levels in patients with proteinuria post cardiac surgery","authors":"Moazaz Rashad Saed , Thikra Hasan Mathkor","doi":"10.1016/j.jpbao.2025.100058","DOIUrl":"10.1016/j.jpbao.2025.100058","url":null,"abstract":"<div><div>Acute kidney injury (AKI) is a prevalent complication following cardiac surgery, affecting both short- and long-term survival rates. Proteinuria serves as an indicator of structural kidney damage and is increasingly recognized as a crucial marker for kidney disease and a risk factor for AKI. Free light chains (FLCs) are being investigated as potential markers for assessing the risk of kidney damage. This study aimed to validate the early detection of AKI by examining FLCs (kappa, lambda, and the kappa/lambda ratio) in serum and saliva samples. Clinical data were collected from 149 patients who underwent cardiac surgery in Baghdad, with 90 providing both saliva and serum samples for FLC evaluation. Patients were categorized based on the severity of proteinuria. Results showed that serum kappa levels were significantly elevated in patients with severe proteinuria compared to those with mild or no proteinuria. Conversely, salivary kappa levels were higher in patients with mild proteinuria than in those with severe or no proteinuria, while salivary lambda levels decreased as proteinuria severity increased. The rise in serum kappa may be attributed to immune system activation and kidney impairment. Both serum and salivary kappa demonstrated strong predictive capabilities for post-surgery AKI prognosis, outperforming lambda and the kappa/lambda ratio based on ROC analysis. The findings suggest that FLCs, particularly kappa, could be valuable in the early detection of AKI following cardiac surgery, highlighting their potential to enhance patient outcomes through proactive monitoring and intervention.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"5 ","pages":"Article 100058"},"PeriodicalIF":0.0,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143280733","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}
Diabetes Mellitus (DM) is among the most widespread multifactorial disorders worldwide, defined by increased plasma glucose levels. Type 2 Diabetes Mellitus (T2DM) is the most prevalent and common form of diabetes mellitus. T2DM is a metabolic condition characterized by abnormal blood glucose levels, insulin resistance in target tissues, and a reduced mass and function of islet β cells. Highlighting the significance of investigating new biomarkers, particularly during the initial stages of development, noncoding RNAs (ncRNAs) have been identified as valuable resources for T2DM. NcRNAs are a class of RNAs found in humans that play significant roles in epigenetics and in regulating post-transcriptional gene expression. Since they function as regulatory molecules, upon base pairing with the mRNA, they exhibit post-transcriptional alterations in the signaling cascade within the cells by regulating the expression of multiple targets simultaneously. Small non-coding RNAs (sncRNAs) and long non-coding RNAs (lncRNAs) are the two primary categories of non-coding RNAs. Several studies have shown that sncRNAs and lncRNAs have evolved as potential biomarkers in T2DM. This review focuses on non-coding RNAs as biomarkers for T2DM and their role in preventing chronic complications.
{"title":"A compendium of noncoding RNAs as biomarkers in Type 2 Diabetes Mellitus","authors":"Manjusha Sita Akella, Angel Mendonca, Thanikes Manikandan, Dhananjay Sateesh, Akshitha Rajesh Swaminathan, Disha Parameshwaran, Manishika Gupta, Sujatha Sundaresan","doi":"10.1016/j.jpbao.2025.100057","DOIUrl":"10.1016/j.jpbao.2025.100057","url":null,"abstract":"<div><div>Diabetes Mellitus (DM) is among the most widespread multifactorial disorders worldwide, defined by increased plasma glucose levels. Type 2 Diabetes Mellitus (T2DM) is the most prevalent and common form of diabetes mellitus. T2DM is a metabolic condition characterized by abnormal blood glucose levels, insulin resistance in target tissues, and a reduced mass and function of islet β cells. Highlighting the significance of investigating new biomarkers, particularly during the initial stages of development, noncoding RNAs (ncRNAs) have been identified as valuable resources for T2DM. NcRNAs are a class of RNAs found in humans that play significant roles in epigenetics and in regulating post-transcriptional gene expression. Since they function as regulatory molecules, upon base pairing with the mRNA, they exhibit post-transcriptional alterations in the signaling cascade within the cells by regulating the expression of multiple targets simultaneously. Small non-coding RNAs (sncRNAs) and long non-coding RNAs (lncRNAs) are the two primary categories of non-coding RNAs. Several studies have shown that sncRNAs and lncRNAs have evolved as potential biomarkers in T2DM. This review focuses on non-coding RNAs as biomarkers for T2DM and their role in preventing chronic complications.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"5 ","pages":"Article 100057"},"PeriodicalIF":0.0,"publicationDate":"2025-01-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143280732","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}
Pub Date : 2025-01-30DOI: 10.1016/j.jpbao.2025.100059
Reem Hasan Obaydo R.H.Obaydo , Abdulsalam Ashkar , Raneem Khayyat , Salem Alhamdan , Hadeel Kallas , Mohammad Kharrat , Amir Alhaj Sakur
A simple, accurate, and environmentally friendly method for determining raw zolmitriptan (ZMT) and its dosage form (tablets) was developed and validated using capillary gas chromatography (GC). Methanol was used to prepare the solutions of the standard and the sample, and instrument parameters were optimized with a programmed temperature ramp ranging from 230 to 290 °C, achieving a total run time of 9.0 min. The retention times for Metronidazole Benzoate (MNZB), the internal standard, and ZMT were found to be 4.89 and 8.11 min, respectively. GC separation was performed with a TRB-5 capillary column (30 m × 0.25 mm, 0.25 μm) with a 0.5 μL injection in splitless mode. The calibration curve was linear when testing a range of concentrations of 6.0–80.0 μg/mL. The limits of detection (LOD) and quantification (LOQ) were determined to be 0.53 and 1.77 μg/mL, respectively, with a correlation coefficient (R²) greater than 0.999. The method proposed was efficiently applicable to analyze pure ZMT and in tablets, showing no interference from other components of the pharmaceutical preparation. Validation of the method was done per ICH guidelines, with all parameters meeting the required acceptance criteria. Additionally, evaluation of the greenness and sustainability of the GC method proposed was performed using AGREE, modified GAPI, and the RGB fast model.
建立了一种简单、准确、环保的测定佐米曲坦（ZMT）原料药及其剂型（片剂）的方法，并利用毛细管气相色谱（GC）进行了验证。用甲醇制备标准品和样品溶液，并在230 ~ 290℃的程序升温范围内优化仪器参数，总运行时间为9.0 min。苯甲硝唑（MNZB）、内标、ZMT的保留时间分别为4.89和8.11 min。色谱柱为TRB-5毛细管柱（30 m × 0.25 mm, 0.25 μm），进样量为0.5 μL，无分裂。在6.0 ~ 80.0 μg/mL范围内，校准曲线呈线性。检测限（LOD）和定量限（LOQ）分别为0.53和1.77 μg/mL，相关系数（R²）均大于0.999。该方法适用于ZMT纯品和片剂的分析，不受制剂中其它成分的干扰。方法的验证按照ICH指南进行，所有参数符合要求的验收标准。此外，采用AGREE、改进GAPI和RGB快速模型对所提出的GC方法的绿色度和可持续性进行了评价。
{"title":"Development of a new green gas chromatographic method for the determination of zolmitriptan in pure and pharmaceutical preparations","authors":"Reem Hasan Obaydo R.H.Obaydo , Abdulsalam Ashkar , Raneem Khayyat , Salem Alhamdan , Hadeel Kallas , Mohammad Kharrat , Amir Alhaj Sakur","doi":"10.1016/j.jpbao.2025.100059","DOIUrl":"10.1016/j.jpbao.2025.100059","url":null,"abstract":"<div><div>A simple, accurate, and environmentally friendly method for determining raw zolmitriptan (ZMT) and its dosage form (tablets) was developed and validated using capillary gas chromatography (GC). Methanol was used to prepare the solutions of the standard and the sample, and instrument parameters were optimized with a programmed temperature ramp ranging from 230 to 290 °C, achieving a total run time of 9.0 min. The retention times for Metronidazole Benzoate (MNZB), the internal standard, and ZMT were found to be 4.89 and 8.11 min, respectively. GC separation was performed with a TRB-5 capillary column (30 m × 0.25 mm, 0.25 μm) with a 0.5 μL injection in splitless mode. The calibration curve was linear when testing a range of concentrations of 6.0–80.0 μg/mL. The limits of detection (LOD) and quantification (LOQ) were determined to be 0.53 and 1.77 μg/mL, respectively, with a correlation coefficient (R²) greater than 0.999. The method proposed was efficiently applicable to analyze pure ZMT and in tablets, showing no interference from other components of the pharmaceutical preparation. Validation of the method was done per ICH guidelines, with all parameters meeting the required acceptance criteria. Additionally, evaluation of the greenness and sustainability of the GC method proposed was performed using AGREE, modified GAPI, and the RGB fast model.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"5 ","pages":"Article 100059"},"PeriodicalIF":0.0,"publicationDate":"2025-01-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143280731","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}
This study incorporates an efficient facile one-pot hydrothermal synthesis of carbon quantum dots (CQD-CK) using the de-oiled copra cake biowaste. The synthesized quantum dots have showed good bioimaging with distinguished fluorescence cell properties with bacterial cultures (Escherichia coli and Streptococcus pyogenes), and yeast cells (Saccharomyces cerevisiae). Throughout the zebrafish's embryonic stages, the synthesized CQD-CK displayed unique fluorescence, indicating the CQD-CKs' increased binding affinities towards the zebrafish's tissues. The optical (UV, PL and FT-IR) and morphological studies (Zeta Potential (ZP), HR-TEM, SEM-EDAX, XRD, Raman spectroscopy) of the synthesized CQD-CK, further confirms the quantum nature of the synthesized CQD-CK (0.262nm through FFT). This work shows that the optical and morphological properties of the synthesized CQD-CK, as well as their synchronized outcomes in the bacterial and live zebrafish embryo and larval imaging, may make them a valuable probe in drug screening, medical research, and toxicological studies.
{"title":"Synthesis of carbon quantum dots from “De-oiled copra cake” by hydrothermal mechanism: In the realm of bioimaging","authors":"Brindha Matharasi Murugan , Suneesha Vazhangodan Abdul Saleem , Gopi Palani Selvan , T. Siva Vijayakumar , Sowmiya Prakash , Gnanadesigan Murugesan","doi":"10.1016/j.jpbao.2025.100060","DOIUrl":"10.1016/j.jpbao.2025.100060","url":null,"abstract":"<div><div>This study incorporates an efficient facile one-pot hydrothermal synthesis of carbon quantum dots (CQD-CK) using the de-oiled copra cake biowaste. The synthesized quantum dots have showed good bioimaging with distinguished fluorescence cell properties with bacterial cultures (<em>Escherichia coli</em> and <em>Streptococcus pyogenes</em>), and yeast cells (<em>Saccharomyces cerevisiae</em>). Throughout the zebrafish's embryonic stages, the synthesized CQD-CK displayed unique fluorescence, indicating the CQD-CKs' increased binding affinities towards the zebrafish's tissues. The optical (UV, PL and FT-IR) and morphological studies (Zeta Potential (ZP), HR-TEM, SEM-EDAX, XRD, Raman spectroscopy) of the synthesized CQD-CK, further confirms the quantum nature of the synthesized CQD-CK (0.262nm through FFT). This work shows that the optical and morphological properties of the synthesized CQD-CK, as well as their synchronized outcomes in the bacterial and live zebrafish embryo and larval imaging, may make them a valuable probe in drug screening, medical research, and toxicological studies.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"5 ","pages":"Article 100060"},"PeriodicalIF":0.0,"publicationDate":"2025-01-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143386967","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}
Pub Date : 2025-01-30DOI: 10.1016/j.jpbao.2025.100056
Ensar Piskin , Zeynep Alakus , Fatma Budak , Ahmet Cetinkaya , Sibel A. Ozkan
Pesticides, used to destroy insects, diseases, and weeds in agricultural products, have increased agricultural activities in countries in recent years. While they have helped reduce the number of pests affecting crops and improved agricultural yields, they have also caused significant environmental hazards. Their toxicity damages the habitats of beneficial creatures, wild animals, and the targeted pests. Additionally, pesticides have a lengthy half-life in the environment, which allows them to build up in species' tissues and go up the food chain, a process known as bioaccumulation and biomagnification. This is a danger to both ecological balance and human health. While a certain amount of excessively used pesticides has a positive effect, increasing amounts remain in the soil and environment as residues. Pesticide residues in the soil pass into foods and fruits. Therefore, there has been a critical need to design electrochemical sensors for sensitive, selective, and rapid analysis of pesticides. Electrochemical sensors offer economical, cost-effective, easy to apply, environmentally friendly, sensitive, and selective advantages for quality and reliable analysis of foods. In addition, many functional nanomaterials are used to increase these sensors' innovative designs and selective and sensitive structures. In this review, the properties, structures, and recent developments regarding the use of the most commonly used nanomaterials in electrochemical sensors designed for pesticide analysis are examined in detail.
Furthermore, the requirements, structural features, and future development of electrochemical sensors that can be prepared cost-effectively and rapidly for sensitive and selective analysis of fruit pesticide residues have been examined and explained in detail. For this reason, the studies in the literature on pesticide analysis in fruits in the last 5 years are summarized, and some studies are explained in detail. Finally, this study will shed light on the studies on fruit pesticide analysis.
{"title":"Nanoparticle-supported electrochemical sensors for pesticide analysis in fruit juices","authors":"Ensar Piskin , Zeynep Alakus , Fatma Budak , Ahmet Cetinkaya , Sibel A. Ozkan","doi":"10.1016/j.jpbao.2025.100056","DOIUrl":"10.1016/j.jpbao.2025.100056","url":null,"abstract":"<div><div>Pesticides, used to destroy insects, diseases, and weeds in agricultural products, have increased agricultural activities in countries in recent years. While they have helped reduce the number of pests affecting crops and improved agricultural yields, they have also caused significant environmental hazards. Their toxicity damages the habitats of beneficial creatures, wild animals, and the targeted pests. Additionally, pesticides have a lengthy half-life in the environment, which allows them to build up in species' tissues and go up the food chain, a process known as bioaccumulation and biomagnification. This is a danger to both ecological balance and human health. While a certain amount of excessively used pesticides has a positive effect, increasing amounts remain in the soil and environment as residues. Pesticide residues in the soil pass into foods and fruits. Therefore, there has been a critical need to design electrochemical sensors for sensitive, selective, and rapid analysis of pesticides. Electrochemical sensors offer economical, cost-effective, easy to apply, environmentally friendly, sensitive, and selective advantages for quality and reliable analysis of foods. In addition, many functional nanomaterials are used to increase these sensors' innovative designs and selective and sensitive structures. In this review, the properties, structures, and recent developments regarding the use of the most commonly used nanomaterials in electrochemical sensors designed for pesticide analysis are examined in detail.</div><div>Furthermore, the requirements, structural features, and future development of electrochemical sensors that can be prepared cost-effectively and rapidly for sensitive and selective analysis of fruit pesticide residues have been examined and explained in detail. For this reason, the studies in the literature on pesticide analysis in fruits in the last 5 years are summarized, and some studies are explained in detail. Finally, this study will shed light on the studies on fruit pesticide analysis.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"5 ","pages":"Article 100056"},"PeriodicalIF":0.0,"publicationDate":"2025-01-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143143188","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}
Pub Date : 2025-01-27DOI: 10.1016/j.jpbao.2025.100055
Tuba Arif , Ahmet Cetinkaya , Mehmet Altay Unal , Esen Bellur Atici , Sibel A. Ozkan
Ibrutinib (IBR) is a Bruton's Tyrosine Kinase (BTK) inhibitor that is being used to treat refractory chronic lymphocytic leukemia (CLL) and mantle cell lymphoma (MCL). Detecting lower levels of IBR in humans could significantly contribute to different areas of research, such as drug delivery. In this work, an electrochemical sensor was designed using a molecularly imprinted polymer on a glassy carbon electrode (GCE) for the selective and sensitive determination of IBR. A polymeric film was obtained on the GCE surface by photopolymerization (PP) method using template molecule IBR, 2-hydroxyethyl methacrylate (HEMA), ethylene glycol dimethacrylate (EGDMA), and 4-aminobenzoic acid (4-ABA). Electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), and scanning electron microscopy (SEM) were used to examine the sensor's morphological and electrochemical characteristics. In addition, the parameters affecting the MIP were optimized. For the first time, a MIP-based electrochemical sensor was designed to determine IBR. Low limit of detection (LOD) and limit of quantification (LOQ) values of 6.13 × 10−14 and 2.04 × 10−13 M were obtained, respectively. The developed sensor detected IBR at least 3 times more selectively than similar substances (pemetrexed (PEM), tofacitinib (TOF), and ruxolitinib (RUX)). IBR detection was investigated in biological samples and pharmaceutical dosage forms. Furthermore, the sensor successfully distinguished IBR from compounds with similar structures, demonstrating great selectivity.
{"title":"Design of a MIP-based electrochemical sensor for sensitive and selective detection of anti-cancer drug ibrutinib in pharmaceutical dosage forms and biological fluids","authors":"Tuba Arif , Ahmet Cetinkaya , Mehmet Altay Unal , Esen Bellur Atici , Sibel A. Ozkan","doi":"10.1016/j.jpbao.2025.100055","DOIUrl":"10.1016/j.jpbao.2025.100055","url":null,"abstract":"<div><div>Ibrutinib (IBR) is a Bruton's Tyrosine Kinase (BTK) inhibitor that is being used to treat refractory chronic lymphocytic leukemia (CLL) and mantle cell lymphoma (MCL). Detecting lower levels of IBR in humans could significantly contribute to different areas of research, such as drug delivery. In this work, an electrochemical sensor was designed using a molecularly imprinted polymer on a glassy carbon electrode (GCE) for the selective and sensitive determination of IBR. A polymeric film was obtained on the GCE surface by photopolymerization (PP) method using template molecule IBR, 2-hydroxyethyl methacrylate (HEMA), ethylene glycol dimethacrylate (EGDMA), and 4-aminobenzoic acid (4-ABA). Electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), and scanning electron microscopy (SEM) were used to examine the sensor's morphological and electrochemical characteristics. In addition, the parameters affecting the MIP were optimized. For the first time, a MIP-based electrochemical sensor was designed to determine IBR. Low limit of detection (LOD) and limit of quantification (LOQ) values of 6.13 × 10<sup>−14</sup> and 2.04 × 10<sup>−13</sup> M were obtained, respectively. The developed sensor detected IBR at least 3 times more selectively than similar substances (pemetrexed (PEM), tofacitinib (TOF), and ruxolitinib (RUX)). IBR detection was investigated in biological samples and pharmaceutical dosage forms. Furthermore, the sensor successfully distinguished IBR from compounds with similar structures, demonstrating great selectivity.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"5 ","pages":"Article 100055"},"PeriodicalIF":0.0,"publicationDate":"2025-01-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143143190","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}
Pub Date : 2025-01-16DOI: 10.1016/j.jpbao.2025.100054
Charlotte De Bleye , Pierre Beckers , Kevser Kemik , Julie Horne , Kenza Lahrichi , Pierre-Yves Sacré , Philippe Hubert , Eric Ziemons
Since 2014, electronic cigarettes must follow the European Directive on tobacco products. In Belgium, the transposition of this directive requires that nicotine-containing e-liquid boosters cannot exceed a concentration of 20 mg mL−1 to ensure consumers safety. Nowadays, accurate analytical methods available to measure nicotine levels in e-liquid products involve chromatography. The development of alternative analytical tools being faster, greener and adaptable to in-field analyses are therefore required. Surface-enhanced Raman scattering is a spectroscopic technique that significantly enhances inherent Raman scattering signals, improving detection limits, when analytes are adsorbed onto metallic nanostructures such as gold nanoparticles (AuNPs). This study introduces new SERS methods for quantifying nicotine in e-liquid boosters using two different Raman spectrophotometers based on a transmission (SETRS) and a backscattering detection mode. The transmission Raman spectrophotometer has a better sample representativity, which is very interesting to perform SERS on liquids samples, and an autosampler offering facilities for routine analyses as a benchtop equipment while the second spectrophotometer was a handheld Raman device allowing to expand the use of the developed SERS method to in-field analyses. These SERS analyses were performed using lab-synthetized AuNps and by adding an isotope-edited internal standards (IEISs) being nicotine-d4 to mitigate some repeatability issues. These methods were finally validated according to the ICH Q2 (R2) guidelines for a working range from 100 to 300 µg L−1 of nicotine concentrations using a total error risk-based approach considering the acceptance limits fixed at 15 % and a risk level of 5 %.
{"title":"Is surface-enhanced Raman spectroscopy (SERS) a good alternative to separation techniques for nicotine dosage in e-liquid boosters?","authors":"Charlotte De Bleye , Pierre Beckers , Kevser Kemik , Julie Horne , Kenza Lahrichi , Pierre-Yves Sacré , Philippe Hubert , Eric Ziemons","doi":"10.1016/j.jpbao.2025.100054","DOIUrl":"10.1016/j.jpbao.2025.100054","url":null,"abstract":"<div><div>Since 2014, electronic cigarettes must follow the European Directive on tobacco products. In Belgium, the transposition of this directive requires that nicotine-containing e-liquid boosters cannot exceed a concentration of 20 mg mL<sup>−1</sup> to ensure consumers safety. Nowadays, accurate analytical methods available to measure nicotine levels in e-liquid products involve chromatography. The development of alternative analytical tools being faster, greener and adaptable to in-field analyses are therefore required. Surface-enhanced Raman scattering is a spectroscopic technique that significantly enhances inherent Raman scattering signals, improving detection limits, when analytes are adsorbed onto metallic nanostructures such as gold nanoparticles (AuNPs). This study introduces new SERS methods for quantifying nicotine in e-liquid boosters using two different Raman spectrophotometers based on a transmission (SETRS) and a backscattering detection mode. The transmission Raman spectrophotometer has a better sample representativity, which is very interesting to perform SERS on liquids samples, and an autosampler offering facilities for routine analyses as a benchtop equipment while the second spectrophotometer was a handheld Raman device allowing to expand the use of the developed SERS method to in-field analyses. These SERS analyses were performed using lab-synthetized AuNps and by adding an isotope-edited internal standards (IEISs) being nicotine-d4 to mitigate some repeatability issues. These methods were finally validated according to the ICH Q2 (R2) guidelines for a working range from 100 to 300 µg L<sup>−1</sup> of nicotine concentrations using a total error risk-based approach considering the acceptance limits fixed at 15 % and a risk level of 5 %.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"5 ","pages":"Article 100054"},"PeriodicalIF":0.0,"publicationDate":"2025-01-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143143654","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}
Pub Date : 2025-01-13DOI: 10.1016/j.jpbao.2025.100053
Mai Oyaide , Takeyuki Akita , Chiharu Ishii , Masashi Mita , Kenji Hamase
The amounts of serine (Ser), threonine (Thr) and allothreonine (aThr) enantiomers in 6 tissues (cerebrum, cerebellum, medulla oblongata, pancreas, liver and kidney) and 2 physiological fluids (plasma and urine) of mice were determined using a highly-selective three-dimensional high-performance liquid chromatographic (3D-HPLC) system. The 3D-HPLC system was composed of reversed-phase (Singularity RP18), anion-exchange (Singularity AX) and chiral separation (Singularity CSP-013S) columns, and the amino acids derivatized with 4-fluoro-7-nitro-2,1,3-benzoxadiazole were determined. To analyze the mouse tissues and physiological fluids, the separation conditions were re-investigated from those reported in our previous study, and the method was validated using the tissue/physiological fluid samples. For Ser, the presence of the d-form could be determined in all the tissues and physiological fluids (1.77 ± 0.09–266.5 ± 11.3 nmol/g or mL). For d-Thr and d-aThr, the presence in the cerebrum and urine was clearly demonstrated (0.28 ± 0.01–1.44 ± 0.56 for d-Thr and 4.63 ± 1.44–6.44 ± 0.36 nmol/g or mL for d-aThr). Trace levels of d-Thr and d-aThr were detected in the other tissues and plasma. The results indicate that the target 3 hydroxy d-amino acids are widely present in mammalian tissues and physiological fluids, and further investigations focusing on their physiological significance are expected.
{"title":"Three-dimensional high-performance liquid chromatographic determination of serine, threonine and allothreonine enantiomers in mouse tissues and physiological fluids","authors":"Mai Oyaide , Takeyuki Akita , Chiharu Ishii , Masashi Mita , Kenji Hamase","doi":"10.1016/j.jpbao.2025.100053","DOIUrl":"10.1016/j.jpbao.2025.100053","url":null,"abstract":"<div><div>The amounts of serine (Ser), threonine (Thr) and allothreonine (aThr) enantiomers in 6 tissues (cerebrum, cerebellum, medulla oblongata, pancreas, liver and kidney) and 2 physiological fluids (plasma and urine) of mice were determined using a highly-selective three-dimensional high-performance liquid chromatographic (3D-HPLC) system. The 3D-HPLC system was composed of reversed-phase (Singularity RP18), anion-exchange (Singularity AX) and chiral separation (Singularity CSP-013S) columns, and the amino acids derivatized with 4-fluoro-7-nitro-2,1,3-benzoxadiazole were determined. To analyze the mouse tissues and physiological fluids, the separation conditions were re-investigated from those reported in our previous study, and the method was validated using the tissue/physiological fluid samples. For Ser, the presence of the <span>d</span>-form could be determined in all the tissues and physiological fluids (1.77 ± 0.09–266.5 ± 11.3 nmol/g or mL). For <span>d</span>-Thr and <span>d</span>-aThr, the presence in the cerebrum and urine was clearly demonstrated (0.28 ± 0.01–1.44 ± 0.56 for <span>d</span>-Thr and 4.63 ± 1.44–6.44 ± 0.36 nmol/g or mL for <span>d</span>-aThr). Trace levels of <span>d</span>-Thr and <span>d</span>-aThr were detected in the other tissues and plasma. The results indicate that the target 3 hydroxy <span>d</span>-amino acids are widely present in mammalian tissues and physiological fluids, and further investigations focusing on their physiological significance are expected.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"5 ","pages":"Article 100053"},"PeriodicalIF":0.0,"publicationDate":"2025-01-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143143189","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}
Pub Date : 2025-01-06DOI: 10.1016/j.jpbao.2025.100052
Shishir Jaikishan , Ramila Mammadova , Rui Chen , Feby Pratiwi , Gabriella Pocsfalvi , Seppo J. Vainio , Susanne K. Wiedmer
Plant-derived nanovesicles (PDNVs) are potential next generation carriers for drug delivery. However, the systemic incorporation of drugs into PDNVs and their quality control still needs extensive research. Previous works showed that Solanum lycopersicum (tomato) fruit is an excellent resource for the high yield manufacturing of tomato PDNVs. Tomato PDNVs have anti-inflammatory activity in vitro which could be further increased by the loading of a lipophilic natural compound, like curcumin. Recently, tolvaptan, a synthetic selective vasopressin V2-receptor antagonist drug was also successfully loaded into tomato PDNVs. In this work, we have advanced the analysis of native and loaded PDNVs and compared them with liposomes using nanoplasmonic sensing (NPS). Tolvaptan was loaded into liposomes composed of phosphatidyl choline (1-palmitoyl-2-oleoyl-sn-glycero-3-phosphocholine or 1,2-dipalmitoyl-sn-glycero-3-phosphocholine) and 1,2-palmitoyl-oleoyl-sn-glycero-3-phosphoserine with and without cholesterol. In addition to NPS, micro differential scanning calorimetry was used to get a deeper understanding of the interactions between tolvaptan and the various liposome compositions. The result of the comparative NPS study showed that tolvaptan can be successfully incorporated both into PDNVs and liposomes of different compositions. The PDNV/tolvaptan and liposome/tolvaptan systems were found to be stable. Due to the low water solubility of tolvaptan, the developed PDNV/tolvaptan or liposome/tolvaptan nanoparticle complexes may present a novel and effective strategy for nanodrug delivery.
{"title":"Nanoplasmonic sensing as a rapid and sensitive methodology to investigate tolvaptan loaded plant-derived nanovesicles and liposomes","authors":"Shishir Jaikishan , Ramila Mammadova , Rui Chen , Feby Pratiwi , Gabriella Pocsfalvi , Seppo J. Vainio , Susanne K. Wiedmer","doi":"10.1016/j.jpbao.2025.100052","DOIUrl":"10.1016/j.jpbao.2025.100052","url":null,"abstract":"<div><div>Plant-derived nanovesicles (PDNVs) are potential next generation carriers for drug delivery. However, the systemic incorporation of drugs into PDNVs and their quality control still needs extensive research. Previous works showed that <em>Solanum lycopersicum</em> (tomato) fruit is an excellent resource for the high yield manufacturing of tomato PDNVs. Tomato PDNVs have anti-inflammatory activity <em>in vitro</em> which could be further increased by the loading of a lipophilic natural compound, like curcumin. Recently, tolvaptan, a synthetic selective vasopressin V2-receptor antagonist drug was also successfully loaded into tomato PDNVs. In this work, we have advanced the analysis of native and loaded PDNVs and compared them with liposomes using nanoplasmonic sensing (NPS). Tolvaptan was loaded into liposomes composed of phosphatidyl choline (1-palmitoyl-2-oleoyl-<em>sn</em>-glycero-3-phosphocholine or 1,2-dipalmitoyl-<em>sn</em>-glycero-3-phosphocholine) and 1,2-palmitoyl-oleoyl-<em>sn</em>-glycero-3-phosphoserine with and without cholesterol. In addition to NPS, micro differential scanning calorimetry was used to get a deeper understanding of the interactions between tolvaptan and the various liposome compositions. The result of the comparative NPS study showed that tolvaptan can be successfully incorporated both into PDNVs and liposomes of different compositions. The PDNV/tolvaptan and liposome/tolvaptan systems were found to be stable. Due to the low water solubility of tolvaptan, the developed PDNV/tolvaptan or liposome/tolvaptan nanoparticle complexes may present a novel and effective strategy for nanodrug delivery.</div></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"5 ","pages":"Article 100052"},"PeriodicalIF":0.0,"publicationDate":"2025-01-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143143653","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}
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