Journal of Pharmaceutical and Biomedical Analysis Open最新文献

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Molecularly imprinted polymers in solid-phase microextraction: Enhancing the analysis of pharmaceutical compounds across diverse sample matrices 固相微萃取中的分子印迹聚合物:加强对不同样品基质中药物化合物的分析
Journal of Pharmaceutical and Biomedical Analysis Open Pub Date : 2024-12-01 Epub Date: 2024-08-08 DOI: 10.1016/j.jpbao.2024.100037
Rafael Oliveira Martins, Almir Custodio Batista Junior, Camila Cíntia Sousa Melo Brito, Yuri Arrates Rocha, Andréa Rodrigues Chaves
{"title":"Molecularly imprinted polymers in solid-phase microextraction: Enhancing the analysis of pharmaceutical compounds across diverse sample matrices","authors":"Rafael Oliveira Martins,&nbsp;Almir Custodio Batista Junior,&nbsp;Camila Cíntia Sousa Melo Brito,&nbsp;Yuri Arrates Rocha,&nbsp;Andréa Rodrigues Chaves","doi":"10.1016/j.jpbao.2024.100037","DOIUrl":"10.1016/j.jpbao.2024.100037","url":null,"abstract":"<div><p>The biomedicine scientific field has made continuous progress, introducing various pharmaceutical compounds to enhance human life. While these advancements bring benefits, the unregulated use of these compounds raises concerns, particularly regarding their presence in the environment and potential adverse effects on human health. Therefore, the assessment of pharmaceutical compounds by analytical strategies is imperative for comprehending and appraising their potential effects and interactions across diverse matrices. In this sense, solid-based microextraction procedures have shed light on the challenging task of evaluating pharmaceutical compounds in complex and diverse samples. Moreover, miniaturized procedures are firmly rooted in the principles of green analytical chemistry, thereby presenting more environmentally friendly approaches than traditional extraction methods. Consequently, significant endeavors have been undertaken to introduce novel sorbent materials that foster a more selective interaction with target analytes. Having this in mind, molecularly imprinted polymers (MIPs) emerge as a solution, providing selective binding sites capable of interacting with the target analyte within a complex sample. The integration of solid-based microextraction procedures with MIPs as sorbent phases has led to significant strides in advancing the evaluation of pharmaceutical compounds in different samples. Hence, this review endeavors to offer a comprehensive overview of the current applications of solid-based microextraction combined with MIPs in the assessment of pharmaceutical compounds across various samples.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"4 ","pages":"Article 100037"},"PeriodicalIF":0.0,"publicationDate":"2024-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2949771X24000136/pdfft?md5=5ce4b0b1b8ca25542029681bdbfea541&pid=1-s2.0-S2949771X24000136-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141978806","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
Validation of a sensitive bioanalytical method for metronidazole extraction from human plasma 验证从人体血浆中提取甲硝唑的灵敏生物分析方法
Journal of Pharmaceutical and Biomedical Analysis Open Pub Date : 2024-06-01 Epub Date: 2024-02-04 DOI: 10.1016/j.jpbao.2024.100025
Krishna Kumar Patel , Valeria Cota , Nicole K. Brogden
{"title":"Validation of a sensitive bioanalytical method for metronidazole extraction from human plasma","authors":"Krishna Kumar Patel ,&nbsp;Valeria Cota ,&nbsp;Nicole K. Brogden","doi":"10.1016/j.jpbao.2024.100025","DOIUrl":"https://doi.org/10.1016/j.jpbao.2024.100025","url":null,"abstract":"<div><p>Metronidazole (MTZ) is a broad-spectrum antibiotic with numerous routes of administration, including topical. Topical application of MTZ gel or cream results in very low systemic absorption, resulting in the need for a sensitive extraction method to quantify plasma concentrations. Currently published methods are not suitable for analysis of plasma concentrations after topical application, as undetectable MTZ concentrations commonly occur. We validated a simple extraction method for MTZ recovery from plasma and quantified it using an LC-MS/MS analytical method. Methods: Plasma samples were spiked with MTZ (0.5 – 5 ng/mL) and internal standard (tinidazole, 2 ng/mL). MTZ was extracted by liquid-liquid extraction using ethyl acetate and acetonitrile mixture (4:1) as the extraction solvent. A quadrupole mass spectrometer interfaced with an Acquity H-Class HPLC was used to quantify MTZ concentrations in positive ion mode. A Kinetix C18 analytical column (150 mm × 4.6 mm i.d., 5 µm particle size) was used for separation. The plasma extraction method was validated for various parameters, including % recovery, precision, accuracy, and stability. Results: The extraction method demonstrated high MTZ recovery, ranging from 93.7 – 97.5%. The calibration curve prepared using MTZ samples extracted from plasma (0.5 – 5 ng/mL) had excellent linearity with R<sup>2</sup> = 0.999. The extracted samples also showed higher autosampler and freeze-thaw stability over a 72-hr period. The mean intra- and inter-day accuracy and precision of the extraction assay ranged from 97 to 101.6% and 2.7 – 4.8% RSD, respectively. The assay was highly efficient, with a limit of quantification (0.53 ± 0.04 ng/mL) lower than previously published methods (≥5 ng/mL). The extraction method was successfully validated using LC-MS/MS and can be used to extract and detect trace amounts of MTZ in plasma after topical application.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"3 ","pages":"Article 100025"},"PeriodicalIF":0.0,"publicationDate":"2024-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2949771X2400001X/pdfft?md5=9b688a9f3a812c65521b6f8b3ea5aeb2&pid=1-s2.0-S2949771X2400001X-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139714996","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
Comparative physicochemical and biological characterization of the similar imiglucerase product Glurazyme® and the originator product Cerezyme® 同类产品 Glurazyme® 和原产地产品 Moscow 的物理化学和生物学特性比较
Journal of Pharmaceutical and Biomedical Analysis Open Pub Date : 2024-06-01 Epub Date: 2023-12-12 DOI: 10.1016/j.jpbao.2023.100024
Maksim Smolov, Serge Taran, Ivan Lyagoskin, Maria Neronova, Maksim Degterev, Rakhim Shukurov
{"title":"Comparative physicochemical and biological characterization of the similar imiglucerase product Glurazyme® and the originator product Cerezyme®","authors":"Maksim Smolov,&nbsp;Serge Taran,&nbsp;Ivan Lyagoskin,&nbsp;Maria Neronova,&nbsp;Maksim Degterev,&nbsp;Rakhim Shukurov","doi":"10.1016/j.jpbao.2023.100024","DOIUrl":"10.1016/j.jpbao.2023.100024","url":null,"abstract":"<div><p>A biosimilar considered as a biomolecule medicinal product that is comparable to a reference medicinal product in terms of the structural, functional, biological, and clinical attributes. Glurazyme® was developed as a biosimilar to Cerezyme® (imiglucerase) and was approved in CIS countries (Russian Federation, Belarus, Kazakhstan) and recently Algeria for the treatment of type 1 and type 3 Gaucher disease. The quality assessment of Glurazyme® was performed in accordance with the Rules for the Study of Biological Medicines of the Eurasian Economic Union harmonized with the ICH comparability guideline and the biosimilar guidelines of the European Medicines Agency and Food and Drug Administration. Extensive side-by-side comparison was employed with state-of-the-art and orthogonal assays designed to interrogate all expected physicochemical and biological activities, including those known to affect the mechanisms of action for imiglucerase. Similarity evaluation was performed on the basis of tolerance intervals determined from about 10 lots of commercial Cerezyme®. Mainly three discrepancies of quality attributes were established concerning oxidized and deamidated forms as well as phosphorylated oligomannose N-glycans reflecting the difference between cultivation and down-stream processes of both medicinal products. Nevertheless, all of them possess a little or no influence on safety and efficacy.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"3 ","pages":"Article 100024"},"PeriodicalIF":0.0,"publicationDate":"2024-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2949771X23000245/pdfft?md5=af72c4a69d296aaef6a235848c9bb9e1&pid=1-s2.0-S2949771X23000245-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139014105","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
Studies on the thermal behavior of sildenafil citrate 枸橼酸西地那非的热行为研究
Journal of Pharmaceutical and Biomedical Analysis Open Pub Date : 2024-06-01 Epub Date: 2024-04-04 DOI: 10.1016/j.jpbao.2024.100028
Francisco V.B. Nascimento, Ana P.G. Ferreira, Rafael T. Alarcon, Éder T.G. Cavalheiro
{"title":"Studies on the thermal behavior of sildenafil citrate","authors":"Francisco V.B. Nascimento,&nbsp;Ana P.G. Ferreira,&nbsp;Rafael T. Alarcon,&nbsp;Éder T.G. Cavalheiro","doi":"10.1016/j.jpbao.2024.100028","DOIUrl":"https://doi.org/10.1016/j.jpbao.2024.100028","url":null,"abstract":"<div><p>Thermal behavior of sildenafil citrate (SC), a vasodilator used in the treatment of both erectile dysfunction (ED) and pulmonary arterial hypertension (PAH) treatment was investigated by thermogravimetry-differential thermal analysis (TGA-DTA), differential scanning calorimetry (DSC), powder X-ray diffraction (PXRD) and evolved gas analysis by thermogravimetry coupled to infrared spectroscopy (TGA-FTIR). Under N<sub>2</sub> and air atmospheres SC remained thermally stable until 180.0 °C, and then decomposed in three steps under N<sub>2</sub> and four steps under air. DSC curves showed two endothermic events at first heating, one related to the dehydration around 63.5 °C and the second event is a concomitant melting-decomposition process (T<sub><em>peak</em></sub> = 199.6 °C). Cold recrystallization was observed during the second heating, with peaks at 119.8 °C and 129.7 °C and melting at 179.7 °C. XRD results for powder collected at 138 °C suggested that the phase formed is the sildenafil free base. TGA-FTIR revealed that the thermal decomposition of SC initiates with release of water, carbon dioxide, and itaconic anhydride, resulting from the decomposition of the citrate counter-ion. Above 303 °C, CO, SO<sub>2</sub>, benzene, ethanol, 1-methylpiperazine, isocyanic acid, and methylamine were identified in the gas phase. Based on these results, a thermal behavior mechanism for sildenafil citrate was proposed.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"3 ","pages":"Article 100028"},"PeriodicalIF":0.0,"publicationDate":"2024-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2949771X24000045/pdfft?md5=134e435dc2a8a6224a704fbdbde2b6aa&pid=1-s2.0-S2949771X24000045-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140539168","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
Ultrasound super resolution imaging for accurate uterus tumor detection and malignancy prediction 超声超分辨率成像用于准确检测子宫肿瘤和预测恶性程度
Journal of Pharmaceutical and Biomedical Analysis Open Pub Date : 2024-06-01 Epub Date: 2024-05-02 DOI: 10.1016/j.jpbao.2024.100029
Ashwini Sawant , Sujata Kulkarni , Milind Sawant
{"title":"Ultrasound super resolution imaging for accurate uterus tumor detection and malignancy prediction","authors":"Ashwini Sawant ,&nbsp;Sujata Kulkarni ,&nbsp;Milind Sawant","doi":"10.1016/j.jpbao.2024.100029","DOIUrl":"https://doi.org/10.1016/j.jpbao.2024.100029","url":null,"abstract":"<div><p>The term ‘tumor’ describes an atypical development of cells that forms a mass inside an organ; depending on the organ's invasive nature and propensity for metastasis, the growth may be benign or malignant. Improving patient outcomes requires the early detection of malignant tumors. Despite its lower resolution and noise problems, ultrasound, which is frequently used to diagnose uterine tumors, is safer and more economical than magnetic resonance imaging (MRI) scans and biopsies. Ultrasound pictures can be processed using methods including denoising, enhancement, segmentation, and feature extraction to get around these restrictions and boost their quality. Enhanced ultrasound images can reach even higher accuracy, cementing them as plausible alternatives to MRI. A comparative analysis of copious relevant image de-speckling, image enhancement, segmentation, and feature extraction methods are carried out. Higher resolution and superior quality, strong segmented real-time ultrasound uterus tumour images are produced by using diffusion-based hybrid filters, Super Resolution Convolutional Neural Networks (SRCNN), and U-net segmentation technique. The Grey Level Co-occurrence Matrix (GLCM) and Discrete Wavelet Transform (DWT) are used to extract textural features. With the help of several machine learning approaches, such as Support Vector Machine (SVM), K-Nearest Neighbour (KNN), and Random Forest classifiers (RFC), the extracted characteristics are immediately sent to classifiers to classify uterus tumours from ultrasound images between benign and malignant. For the categorization of uterine tumors, the RFC classifier outperformed the other classifiers. The viability of cancer detection using ultrasound pictures is significantly strengthened by the suggested machine learning methodology. Multiple hospitals provided data on ultrasound pictures of uterine tumors, which were used to develop the model and obtain the prediction findings. A radiologist with 17 years of expertise in diagnostic radiology further assessed this dataset. We could produce high-quality ultrasonic real-time images of uterine tumor datasets with the suggested machine learning model at a 97.8 % accuracy rate utilizing RFC.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"3 ","pages":"Article 100029"},"PeriodicalIF":0.0,"publicationDate":"2024-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2949771X24000057/pdfft?md5=b0ec160d7302bc75f048a1a6eb6c44b8&pid=1-s2.0-S2949771X24000057-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140918528","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
Mitigating matrix effects for LC-MS/MS quantification of nitrosamine impurities in rifampin and rifapentine 减轻基质效应以实现利福平和利福喷丁中亚硝胺杂质的 LC-MS/MS 定量
Journal of Pharmaceutical and Biomedical Analysis Open Pub Date : 2024-06-01 Epub Date: 2024-02-24 DOI: 10.1016/j.jpbao.2024.100027
Qiyao Li , Qun Xu , Nadine Lo , Allan T. Leeks Jr. , Mark Han , Marcela Nefliu , John T. Simpson , Jennifer L. Belsky
{"title":"Mitigating matrix effects for LC-MS/MS quantification of nitrosamine impurities in rifampin and rifapentine","authors":"Qiyao Li ,&nbsp;Qun Xu ,&nbsp;Nadine Lo ,&nbsp;Allan T. Leeks Jr. ,&nbsp;Mark Han ,&nbsp;Marcela Nefliu ,&nbsp;John T. Simpson ,&nbsp;Jennifer L. Belsky","doi":"10.1016/j.jpbao.2024.100027","DOIUrl":"https://doi.org/10.1016/j.jpbao.2024.100027","url":null,"abstract":"<div><p>Since the discovery of potentially mutagenic nitrosamine impurities in pharmaceuticals in 2018, liquid chromatography-mass spectrometry (LC-MS) methods have been widely applied for the trace level quantification of nitrosamines. As more nitrosamines and drug samples are analyzed, method accuracy is increasingly recognized as a major analytical challenge. Matrix effects can have a significant adverse impact on method accuracy but have not attracted much attention in nitrosamine quantification literature. In this study, we observed severe matrix effects when adapting LC-MS method conditions from a published and validated method for the analysis of nitrosamines in tuberculosis drugs. Several approaches were explored to mitigate these matrix effects, including using stable isotope-labeled internal standards, modifying LC conditions and sample concentration, and quantifying with standard addition instead of an external calibration method. The results underscore the importance of monitoring matrix effects and validating nitrosamine quantification procedures for specific sample matrices. Finally, two LC-MS/MS methods are presented with validation data for the quantification of 1-methyl-4-nitrosopiperazine (MNP) in rifampin and 1-cyclopentyl-4-nitrosopiperazine (CPNP) in rifapentine and revealed high nitrosamine levels in the tested samples that far exceeded recommended acceptable intake limits.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"3 ","pages":"Article 100027"},"PeriodicalIF":0.0,"publicationDate":"2024-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2949771X24000033/pdfft?md5=943d4b0163ce944a7c98d3f4e92c1d2d&pid=1-s2.0-S2949771X24000033-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139987016","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
Synthesis of biowaste-derived nanostructured material for the nanomolar detection of glucose: Biological sample analysis 用于纳摩尔葡萄糖检测的生物废料纳米结构材料的合成:生物样品分析
Journal of Pharmaceutical and Biomedical Analysis Open Pub Date : 2024-06-01 Epub Date: 2024-02-21 DOI: 10.1016/j.jpbao.2024.100026
Shweta J. Malode , Shireesha Bilagi , Nagaraj P. Shetti
{"title":"Synthesis of biowaste-derived nanostructured material for the nanomolar detection of glucose: Biological sample analysis","authors":"Shweta J. Malode ,&nbsp;Shireesha Bilagi ,&nbsp;Nagaraj P. Shetti","doi":"10.1016/j.jpbao.2024.100026","DOIUrl":"https://doi.org/10.1016/j.jpbao.2024.100026","url":null,"abstract":"<div><p>Glucose electro-oxidation in an alkaline media was investigated using an electrode composed of carbon paste and sugarcane bagasse activated carbon (SBAC). The SBAC was prepared using an easy, affordable, and environmental friendly process. The porous activated carbon was produced using sugarcane bagasse through a pre-treatment process that involved carbonization at 650 °C and K<sub>2</sub>CO<sub>3</sub>. X-ray diffraction (XRD) was used to observe the formation of carbon crystallites during activation at higher temperatures. The Fourier-transform infrared (FTIR) spectrum shows functional groups that are present in the carbon material. The carbon sample's morphology was evaluated using scanning electron microscope (SEM). The surface roughness was studied using atomic force microscopy (AFM). Porous activated carbon derived from sugarcane bagasse was carefully mixed into electrode components such as graphite powder and mineral oil for glucose (GLS) detection. For precise GLS detection, the SBACs were employed as non-enzymatic electrochemical sensor probes in their as-prepared condition. According to the electrochemical experiments, the constructed sensor shows exceptional electrochemical performance towards glucose oxidation, including excellent selectivity, a low detection limit, good sensitivity, and a wide linear range. Investigation has been conducted on the oxidation of GLS in alkaline solutions with varying concentrations of halide ions such as iodide and chloride. The GLS oxidation peak current increased the performance of a SBAC modified electrode was compared to that of a bare carbon paste electrode (CPE). The role of sensitivity in minimizing halide poisoning is significant. The risk of poisoning is increased if iodide &gt; chloride. As the modified electrode's voltage changes in a chloride solution containing glucose, the peak current gradually reduces. The redesigned electrode that is currently in use as a consequence not only promotes glucose oxidation but also shows strong resistance to electrode poisoning caused by halides. The sensitive and targeted SBAC/CPE has also improved its reliability while evaluating samples of human serum, urine, and breast milk.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"3 ","pages":"Article 100026"},"PeriodicalIF":0.0,"publicationDate":"2024-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2949771X24000021/pdfft?md5=5af6905d7f946aac73c3319cc9e20fb4&pid=1-s2.0-S2949771X24000021-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139987015","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
Formic acid-aided sample preparation method for sensitive and simultaneous analysis of eight nitrosamines in poorly-water soluble pharmaceutical drugs using liquid chromatography–ultraviolet detection 液相色谱-紫外检测法测定难水溶性药物中8种亚硝胺的甲酸辅助制样方法
Journal of Pharmaceutical and Biomedical Analysis Open Pub Date : 2023-12-01 Epub Date: 2023-10-20 DOI: 10.1016/j.jpbao.2023.100020
Eiichi Yamamoto, Hitomi Kan-no, Daisuke Ando, Tamaki Miyazaki, Tatsuo Koide, Ken-ichi Izutsu, Yoji Sato
{"title":"Formic acid-aided sample preparation method for sensitive and simultaneous analysis of eight nitrosamines in poorly-water soluble pharmaceutical drugs using liquid chromatography–ultraviolet detection","authors":"Eiichi Yamamoto,&nbsp;Hitomi Kan-no,&nbsp;Daisuke Ando,&nbsp;Tamaki Miyazaki,&nbsp;Tatsuo Koide,&nbsp;Ken-ichi Izutsu,&nbsp;Yoji Sato","doi":"10.1016/j.jpbao.2023.100020","DOIUrl":"10.1016/j.jpbao.2023.100020","url":null,"abstract":"<div><p>There has been a growing concern over the contamination of pharmaceutical products with nitrosamines (NAs) such as <em>N</em>-nitrosodimethylamine (NDMA). To quantify NA levels in drugs using reversed-phase liquid chromatography (LC), the sample solution should achieve a high drug concentration to detect trace NAs, and an appropriate amount of hydrophilic NAs should be retained. However, these are difficult to achieve, and no suitable method has yet been developed. The present study was the first to develop a sample preparation method to achieve this by combining drugs with formic acid (FA), followed by the removal of active pharmaceutical ingredients (APIs) from samples via crystallization. This method was successfully applied for the sensitive quantification of eight NAs in poorly water-soluble acidic atorvastatin (ATS) and basic itraconazole (ITC) via LC–ultraviolet (LC-UV) detection. The removal rate of ITC via recrystallization exceeded 99.96 %, whereas most NAs remained as solutes. Assuming that the enhancement in ITC solubility directly translates to heightened analytical sensitivity, a &gt; 100-fold increase in sensitivity was attained compared to conventional methodologies. This sample preparation method would be applicable to other poorly water-soluble drugs, contributing to the control of NA content in various formulations to realize the safe delivery of pharmaceuticals to patients.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"2 ","pages":"Article 100020"},"PeriodicalIF":0.0,"publicationDate":"2023-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2949771X23000208/pdfft?md5=7d42ede05957e2e87dab21117535373b&pid=1-s2.0-S2949771X23000208-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135965851","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
Development of an enantioselective three-dimensional HPLC system for the determination of alanine, valine, isoleucine, allo-isoleucine and leucine in human plasma and urine 建立测定血浆和尿液中丙氨酸、缬氨酸、异亮氨酸、异亮氨酸和亮氨酸的对映选择性三维高效液相色谱系统
Journal of Pharmaceutical and Biomedical Analysis Open Pub Date : 2023-12-01 Epub Date: 2023-06-15 DOI: 10.1016/j.jpbao.2023.100013
Yuri Nagata , Takeyuki Akita , Chiharu Ishii , Mai Oyaide , Masashi Mita , Tomomi Ide , Kenji Hamase
{"title":"Development of an enantioselective three-dimensional HPLC system for the determination of alanine, valine, isoleucine, allo-isoleucine and leucine in human plasma and urine","authors":"Yuri Nagata ,&nbsp;Takeyuki Akita ,&nbsp;Chiharu Ishii ,&nbsp;Mai Oyaide ,&nbsp;Masashi Mita ,&nbsp;Tomomi Ide ,&nbsp;Kenji Hamase","doi":"10.1016/j.jpbao.2023.100013","DOIUrl":"https://doi.org/10.1016/j.jpbao.2023.100013","url":null,"abstract":"<div><p>A three-dimensional (3D) HPLC system was designed/developed for the discriminative determination of aliphatic chiral amino acids, namely, alanine (Ala), valine (Val), isoleucine (Ile), <em>allo</em>-Ile (aIle) and leucine (Leu), in human physiological fluids. These aliphatic amino acid enantiomers are expected to be new physiologically active molecules and/or biomarkers in mammals. Among these aliphatic amino acids, the structural chain isomers of Leu (Ile/aIle/Leu) have similar chemical-physical properties, and the analytical method for these aliphatic amino acids is required to be highly enantio- and chemo-selective. In the present study, a reversed-phase column (Singularity RP18, first dimension) and a mixed-mode column (Singularity MX-103, second dimension) were utilized to separate these aliphatic amino acids as their scalemic mixtures, then chiral separations were performed using a Pirkle-type enantioselective column (Singularity CSP-001S) in the third dimension. By using the 3D-HPLC system, these aliphatic amino acid enantiomers were completely discriminated, and the analysis of these aliphatic chiral amino acids in the human plasma and urine was successfully carried out. The obtained amounts of the aliphatic amino acids (and %D value, the percentage of <span>D</span>-form to D + L forms) in the human plasma were 2.1 µM (0.5%) for <span>D</span>-Ala, and trace/not-detected for the other <span>D</span>-forms. In human urine, the values were 102.0 µM (24.7%) for D-Ala, 2.0 µM (3.4%) for D-Val, 2.3 µM (10.8%) for D-aIle (%D value of D-aIle was calculated using D-aIle and <span>L</span>-Ile) and 3.3 µM (5.5%) for D-Leu. The present 3D-HPLC system is a powerful and well validated tool for the simultaneous determination of aliphatic amino acid enantiomers, and further biological and clinical studies are expected.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"2 ","pages":"Article 100013"},"PeriodicalIF":0.0,"publicationDate":"2023-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49879896","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
Expression analysis of p50-associated COX-2 extragenic RNA and NF-Kappa B Interacting long non-coding RNA in multiple sclerosis patients 多发性硬化症患者p50相关COX-2外基因RNA和NF-Kappa B相互作用长链非编码RNA的表达分析
Journal of Pharmaceutical and Biomedical Analysis Open Pub Date : 2023-12-01 Epub Date: 2023-08-06 DOI: 10.1016/j.jpbao.2023.100017
Zeinab Shirvani-Farsani , Mina Rezaei , Zahra Abedi Kichi , Mehrdad Behmanesh , Shirin Farivar
{"title":"Expression analysis of p50-associated COX-2 extragenic RNA and NF-Kappa B Interacting long non-coding RNA in multiple sclerosis patients","authors":"Zeinab Shirvani-Farsani ,&nbsp;Mina Rezaei ,&nbsp;Zahra Abedi Kichi ,&nbsp;Mehrdad Behmanesh ,&nbsp;Shirin Farivar","doi":"10.1016/j.jpbao.2023.100017","DOIUrl":"https://doi.org/10.1016/j.jpbao.2023.100017","url":null,"abstract":"<div><p>Inflammatory long non-coding RNAs (lncRNAs) including PACER (p50-associated COX-2 extragenic RNA) and NKILA (NF-Kappa B Interacting long non-coding RNA) and have recently emerged as essential regulators in immune and inflammation pathways in patients with multiple sclerosis (MS), which have possible worthiness as diagnostic, prognostic, and therapeutic targets. In the current study, we aimed to evaluate the expressions of PACER, NKILA lncRNAs, CTCF (CCCTC-binding factor), and NF-κB in the PBMC (peripheral blood mononuclear cells) from MS patients and control subjects. We detected the expression levels of PACER, CTCF, NKILA, and NF-kB using real-time PCR in 39 MS patients and 37 healthy controls. The findings show that the expression levels of PACER lncRNA and CTCF, but not NKILA lncRNA and NF-κB, have significantly decreased in MS patients compared to the controls, so they are probably involved in MS pathogenesis. Notably, the area under the ROC curve for PACER and CTCF was up to 0.80 and 0.68, respectively. Based on these observations, the PACER and CTCF had been shown to have the best efficiency in the discrimination of disease status between MS patients and healthy controls. A low expression level of CTCF was correlated with PACER lncRNA and NF-KB expression levels as well as some factors including disease duration, age, and EDSS. Altogether, these results demonstrate that PACER lncRNA and CTCF were potentially related to the MS risk. However, further functional investigations are required to confirm the roles of these genes in the etiology of MS.</p></div>","PeriodicalId":100822,"journal":{"name":"Journal of Pharmaceutical and Biomedical Analysis Open","volume":"2 ","pages":"Article 100017"},"PeriodicalIF":0.0,"publicationDate":"2023-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49879897","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
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