Journal of Chromatography B最新文献

{"title":"Identification, synthesis, isolation, and characterization of formulation related degradation impurity of Cefadroxil Oral suspension","authors":"Sunil Ramrao Murkute ,&nbsp;Surenehalli Gowdra Vasantharaju ,&nbsp;Girij P. Singh ,&nbsp;Krishnamurthy Bhat ,&nbsp;Himanshu M. Godbole ,&nbsp;Pritesh R. Upadhyay ,&nbsp;Anurag Trivedi","doi":"10.1016/j.jchromb.2025.124537","DOIUrl":"10.1016/j.jchromb.2025.124537","url":null,"abstract":"<div><div>Cefadroxil is an orally active, first-generation cephalosporin antibiotic utilized in the treatment of bronchitis, pharyngitis, tonsillitis, urinary tract infections, uncomplicated skin infections, bones, and joints (de Marco and Salgado, 2017 [<span><span>1</span></span>]). Cefadroxil for oral suspension is formulated as dry powder for oral suspension. After reconstitution during 14 days storage, we observed an unknown impurity at relative retention time (RRT) 1.29 in cefadroxil oral suspension. The observed level of an unknown impurity was greater than 0.1 % in high-performance liquid chromatography (HPLC) analysis. The present work is focused on the identification, synthesis, and characterization of the unknown impurity by employing several sophisticated analytical techniques. Such as High-resolution mass spectroscopy (HRMS), One dimensional (1D) and two dimensional (2D) nuclear magnetic resonance spectroscopy.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1256 ","pages":"Article 124537"},"PeriodicalIF":2.8,"publicationDate":"2025-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143601359","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Profiling neuroactive steroids in pregnancy. A non-derivatised liquid chromatography tandem mass spectrometry method for the quantitation of allopregnanolone and four related isomers in maternal serum.","authors":"Edward Hinchliffe ,&nbsp;Alexander Heazell","doi":"10.1016/j.jchromb.2025.124541","DOIUrl":"10.1016/j.jchromb.2025.124541","url":null,"abstract":"<div><div>Neuroactive steroids are metabolites of progesterone, synthesised during pregnancy by the placenta. Here, we describe development of a novel liquid chromatography tandem mass spectrometry (LC-MS/MS) assay for quantitation of allopregnanolone, pregnanolone, isopregnanolone, epipregnanolone and allopregnan-20α-ol-3-one in maternal serum. Following addition of deuterated internal standards, 200 μL of serum was subjected to solid phase extraction. Chromatography was performed using a pentafluorophenyl column, and LC-MS/MS on a Sciex 6500+. Sample injection volume was 20 μL, and injection-to-injection time 10.0 min. The assay was validated according to published guidelines; assay linearity and lower limit of quantification were suitable for analysis of each steroid in maternal serum, for all analytes mean recoveries were 100 % ± 15 %, intra- and inter-assay imprecision &lt;15 %, and matrix effects negligible, and specificity experiments confirmed nil interference from a wide range of endogenous metabolites of progesterone. The method was applied to human serum samples obtained from a large cohort of third trimester pregnancies which were subsequently characterised by normal fetal and maternal outcomes, and relationships between maternal neuroactive steroid concentrations and fetal gestational age assessed. Positive correlations between maternal serum concentration and fetal gestational age were observed for isopregnanolone, allopregnanolone and allopregnan-20α-ol-3-one. The LC-MS/MS method offers significant advantages over previously published approaches for quantitation of neuroactive steroids in human maternal serum, notably obviating the need for derivatisation, whilst achieving exceptional specificity. Characterisation of normal maternal neuroactive steroid concentrations will aid future research as dysregulated placental progesterone metabolism is observed in pregnancies with poor outcomes.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1256 ","pages":"Article 124541"},"PeriodicalIF":2.8,"publicationDate":"2025-02-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143549621","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Optimizing nuclease treatment to enhance anion exchange chromatography of HIV-derived virus-like particles","authors":"M.S. von Elling-Tammen ,&nbsp;F. Taft ,&nbsp;V. Thom ,&nbsp;J. Stitz ,&nbsp;S. Barbe ,&nbsp;A. Krause","doi":"10.1016/j.jchromb.2025.124539","DOIUrl":"10.1016/j.jchromb.2025.124539","url":null,"abstract":"<div><div>Residual host cell chromatin imposes numerous challenges on purifying HIV-derived enveloped virus-like particles (VLPs) using anion-exchange chromatography (AEX). According to FDA guidelines, DNA must be reduced to less than 10 ng per dose at a fragment size of less than 200 bp. To prove the fulfillment of these quality criteria, methods for the qualitative and quantitative analysis of DNA fragments must be applied and adapted to chromatin. DNA and chromatin impede the purification of HIV VLPs with AEX, co-eluting in the same fractions as the VLPs. Although nuclease treatments can be employed, the chromatin structure can shield DNA from nuclease activity. To address these challenges, we adjusted our analytical focus on characterizing the chromatin in our clarified HIV VLP supernatant. We identified two DNA subpopulations: a main large fragment population and a minor population consisting of short fragments below 200 bp. Our findings demonstrated that the larger DNA fragments are the primary issue in our process, as they co-elute with the desired VLPs. To remove the long DNA fragment population, we optimized the nuclease treatment using a Design of Experiment approach to digest the DNA despite the tight chromatin structure. The nucleases Benzonase, Denarase, and M-SAN efficiently digested the DNA removing over 90 % of the DNA. By shredding the long DNA fragments before the AEX step, we successfully separated the HIV VLPs from the remaining short DNA fragments. Combined with nuclease treatment, AEX membrane chromatography offers an efficient single-step purification platform for HIV VLP-based vaccines and other therapeutics.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1256 ","pages":"Article 124539"},"PeriodicalIF":2.8,"publicationDate":"2025-02-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143579713","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Rapid and sensitive HPLC with fluorescence detection method for quantifying selpercatinib in liver microsomes and rat plasma: Implications for drug-drug interaction studies","authors":"Aref L. Zayed ,&nbsp;Aysheh M. Alshekhhossin ,&nbsp;Omar M. Al Kilani ,&nbsp;Sana'a A. Jaber ,&nbsp;Leen L. Dawood ,&nbsp;Jomana Al Hroot ,&nbsp;Kawthar Z. Alzarieni","doi":"10.1016/j.jchromb.2025.124542","DOIUrl":"10.1016/j.jchromb.2025.124542","url":null,"abstract":"<div><div>Selpercatinib (RETEVMO®) is a selective anticancer agent recently approved for thyroid and non-small cell lung cancer. Reliable analytical methods are essential for investigating its potential drug interactions. In this study, the fluorescence properties of selpercatinib were exploited for the first time to develop a sensitive high-performance liquid chromatography with fluorescence detection (HPLC-FLD) method to quantify selpercatinib in human and rat liver microsomes and rat plasma. The method was successfully validated according to M10 guidelines demonstrating excellent accuracy, precision, selectivity, and sensitivity across a concentration range of (50–2000) ng/mL in plasma samples, with a short run time of less than 4 min. The method was applied to metabolic stability studies, where selpercatinib exhibited moderate intrinsic clearance (CL_int) in human liver microsomes (CL_int of 44.9 μL/min/mg), low clearance in female rat liver microsomes (CL_int 10.6 μL/min/mg), and nearly no depletion in male rat liver microsomes. After treatment with dexamethasone, the clearance of selpercatinib was enhanced in both female and male rat liver microsomes, suggesting potential drug-drug interaction. Dexamethasone-treated female rat liver microsomes showed clearance similar to human liver microsomes, indicating their suitability as a surrogate model for studying human metabolism <em>in vitro</em>. Additionally, the inhibitory effect of myricetin on selpercatinib metabolism was comparable in both human and dexamethasone-treated female rat liver microsomes, with IC₅₀ values of 9.3 μM and 10.9 μM, respectively. These findings suggest the need to investigate these potential drug interactions in clinical settings, as they may affect selpercatinib efficacy and toxicity. This HPLC-FLD method offers a rapid, sensitive, and cost-effective alternative to LC-MS/MS for studying pharmacokinetics in various <em>in vitro</em> and <em>in vivo</em> models.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1256 ","pages":"Article 124542"},"PeriodicalIF":2.8,"publicationDate":"2025-02-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143592420","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Current developments and trends in hybrid extraction techniques for green analytical applications in natural products","authors":"Navratan Soni,&nbsp;Mukul Yadav,&nbsp;Malarvannan. M,&nbsp;Dhanashree Sharma,&nbsp;David Paul","doi":"10.1016/j.jchromb.2025.124543","DOIUrl":"10.1016/j.jchromb.2025.124543","url":null,"abstract":"<div><div>Natural product extraction has advanced significantly due to the growing need for environmentally friendly and sustainable analytical techniques. The medicinal benefits of natural products are gaining worldwide recognition. This shift emphasizes the need for sustainable extraction methods, as traditional organic solvents can negatively impact biodiversity. This review looks at new green extraction methods such as pressurized liquid extraction, ultrasound-assisted extraction, microwave-assisted extraction, and supercritical fluid extraction. The overview describes the main goals, workings, and extraction principles of these techniques, which are used to extract phytochemicals from various plant sources. Additionally covered is how green solvents, more especially bio-based and deep eutectic solvents, can enhance the sustainability of these techniques. This review examines the developments in synergistic extraction, emphasizing how these hybrid techniques can be used to isolate a variety of natural products, including polyphenols, alkaloids, essential oils, and more. It also emphasizes how crucial these techniques are to the development of high-performance, environmentally friendly analytical platforms for the use of natural products. The recent uses of these extraction techniques are covered in this review. Despite the positive results, standardization, selectivity, scalability, and economic viability issues must be recognized and addressed.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1256 ","pages":"Article 124543"},"PeriodicalIF":2.8,"publicationDate":"2025-02-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143549622","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Integration of UHPLC-MS and mass spectrometry imaging techniques revealed the protective mechanism of Gushudan in postmenopausal osteoporosis rats via branched-chain amino acid metabolism based on the ‘kidney-bone’ axis","authors":"Mengxin Ren,&nbsp;Yajing Wang,&nbsp;Yue Yuan,&nbsp;Hailing Du,&nbsp;Qinghua Liang,&nbsp;Feng Qin,&nbsp;Zhili Xiong","doi":"10.1016/j.jchromb.2025.124540","DOIUrl":"10.1016/j.jchromb.2025.124540","url":null,"abstract":"<div><div>According to the theory of traditional Chinese medicine, the kidney is regarded as governing the bones and dominating the storage of essence. Gushudan (GSD) is a traditional Chinese medicine prescription that has the effects of strengthening bone and nourishing the kidney. However, the mechanism of action of GSD in preventing postmenopausal osteoporosis (PMOP) rats based on the ‘kidney-bone’ axis remains to be further systematically investigated. In this study, an integrated kidney metabolomics method based on three MS detection modes of UHPLC-HRMS, UHPLC-MS/MS and AFADESI-MSI was developed to reveal the protective mechanism of GSD in PMOP rats. Firstly, the non-targeted metabolomics was investigated to comprehensively explore the metabolic changes in the kidneys of PMOP rats based on the UHPLC-Q-Orbitrap HRMS. Subsequently, UHPLC-MS/MS targeted metabolomics and Mass Spectrometry Imaging (MSI) techniques were combined to elucidate the preventive mechanism of GSD on PMOP through branched-chain amino acid (BCAA) metabolism. The results of the non-targeted metabolomics demonstrated that GSD significantly modulated the levels of 67 potential biomarkers, including leucine and valine, which are primarily involved in amino acid metabolism. Specifically, BCAA metabolism is notably enriched in amino acid metabolism. Compared to the control group, it was found that the levels of BCAAs were decreased and α-branched-chain keto acids (BCKAs) were increased in the model groups in the targeted metabolomics study. Moreover, MSI results showed that the changes in BCAAs content were mainly concentrated in the renal cortex. This finding confirmed the metabolic disorders of BCAA in the renal cortex of PMOP rats, and that GSD had a significant regulatory effect on this disorder. In conclusion, this study integrated three mass spectrometry techniques that validate and complement each other to revealed the anti-osteoporostic mechanism of GSD in PMOP rats and to elucidate the modern scientific connotation of the ‘kidney-bone’ axis based on the BCAA metabolism.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1256 ","pages":"Article 124540"},"PeriodicalIF":2.8,"publicationDate":"2025-02-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143512226","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Pharmacokinetics comparison of seven active components after oral administration of Zhizhu pill using raw and processed Rhizoma Atractylodis Macrocephalae","authors":"Liu Si-qi ,&nbsp;Zheng Wei ,&nbsp;Zang Bin-ru ,&nbsp;Wu Hao ,&nbsp;Zhang Ke ,&nbsp;Liu Xiang ,&nbsp;Yuan Chu ,&nbsp;Zhao Qi-miao ,&nbsp;Shan Guo-shun","doi":"10.1016/j.jchromb.2025.124521","DOIUrl":"10.1016/j.jchromb.2025.124521","url":null,"abstract":"&lt;div&gt;&lt;div&gt;Zhizhu pills (ZZP) is a Traditional Chinese Medicine that has been extensively applied in the treatment of spleen deficiency and constipation for many years. As a commonly used prescription in Traditional Chinese medicine, there had been a controversy over whether to use raw Rhizoma Atractylodis Macrocephalae (RRAM) or Bran-Fired Rhizoma Atractylodis Macrocephalae (BRAM) in ZZP. In this study, a specific, sensitive, fast and accurate liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was developed to analyze the main active components in ZZP. It was used to determine the compound of Atractylenolide I, Atractylenolide III, Synephrine, Nuciferine, Narirutin, Naringin and Hesperidin in rat various biological matrices (plasma, tissue, urine and feces). The liquiritin was used as the internal standard. All the biological samples were prepared using a simple protein precipitation with acetonitrile and methanol (1:1, &lt;em&gt;V&lt;/em&gt;/V). A waters UPLC HSS T3 (100 × 2.1 mm, 1.8 μm) column was used in this research. The mobile phase consisting of 0.1 % aqueous formic acid (A)-0.1 % formic acid in acetonitrile (B) was employed to separate seven components from endogenous interferences. The components were detected with a triple quadrupole mass spectrometer using positive and negative ion multiple reaction monitoring (MRM) mode. The newly developed method was successfully applied to investigate the pharmacokinetics, tissue distribution and excretion of seven components after intragastric administration ZZP which was composed with RRAM or BRAM in rats. The pharmacokinetic results indicated that seven active components can be quickly absorbed and had undergone the enterohepatic circulation. It could also indicate higher &lt;em&gt;C&lt;/em&gt;&lt;sub&gt;max&lt;/sub&gt; of Nuciferine, Narirutin, Naringin and Hesperidin in the plasma after intragastric administration ZZP compose of BRAM than RRAM. In tissue distribution, the seven active components in ZZP were mainly distributed in the stomach, large intestine and small intestine. It could indicate a lower &lt;em&gt;C&lt;/em&gt;&lt;sub&gt;max&lt;/sub&gt; of Atractylenolide I, Atractylenolide III in the stomach, large intestine and small intestine after intragastric administration ZZP compose of BRAM compared to RRAM. It could also indicate higher Cmax of Narirutin, Naringin, and Synephrine in the stomach, large intestine and small intestine after intragastric administration ZZP compose of BRAM than RRAM. The results of the excretion study showed that the total urinary excretion rate of the 7 active components at 48 h was lower after intragastric administration ZZP compose of BRAM than RRAM. Meanwhile, the total fecal excretion rate of the 7 active components was higher after intragastric administration ZZP compose of BRAM than RRAM. The pharmacokinetics, tissue distribution and excretion characteristics of seven active components in ZZP were first revealed. It also used to compare the difference of ZZP compose of BRAM than RRAM in the pha","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1256 ","pages":"Article 124521"},"PeriodicalIF":2.8,"publicationDate":"2025-02-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143487926","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Serum untargeted metabolomics combined with mouse models reveals potential mechanisms of ChengShu QingChu decoction for the treatment of vitiligo","authors":"Xiangran Liu ,&nbsp;Abudureyimu Alimujiang ,&nbsp;Wenjing Wei ,&nbsp;Dengqiu Xu ,&nbsp;Tuerxun Wufuer ,&nbsp;Julaiti Abuduwayiti ,&nbsp;Shixia Huo ,&nbsp;Zhijian Li","doi":"10.1016/j.jchromb.2025.124538","DOIUrl":"10.1016/j.jchromb.2025.124538","url":null,"abstract":"<div><div>To illustrate the potential immunological mechanisms of ChengShu QingChu Decoction (CSQC) in vitiligo treatment. An untargeted metabolomic approach was used to detect serum metabolites in 30 patients with progressive vitiligo. Annotation of the differential metabolites were performed using MetaboAnalyst 5.0 and the KEGG database. In addition, 58 Hub genes associated with metabolic pathways were obtained from the GSEA and KEGG databases, and functional enrichment for Hub genes. Finally, it was validated by a mouse model. 102 down-regulated and 86 up-regulated metabolites were detected in serum. The main metabolic pathways enriched for differential metabolites were sphingolipid metabolism and glycerophospholipid metabolism, and the signaling pathways included PI3K-Akt and JAK-STAT signaling pathways, and immune cells included CD56 bright natural killer cell and Central memry CD8 T cell. In the mouse model, a significant decrease in the number of CD8⁺T cells as well as a decrease in the mRNA expression of JAK1, JAK2, and STAT1 was observed in addition to a trend toward increased melanocytes after drug treatment. This study utilizes metabolomics and bioinformatics analyses, combined with in vivo experimental validation, to elucidate the potential mechanism of CSQC in the treatment of vitiligo.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1256 ","pages":"Article 124538"},"PeriodicalIF":2.8,"publicationDate":"2025-02-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143549706","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Finger-prick blood sampling using volumetric absorptive microsampling (VAMS) method for monitoring the main (poly)phenolic metabolites in human blood after barley biscuit intake","authors":"María-Engracia Cortijo-Alfonso ,&nbsp;Silvia Yuste ,&nbsp;Carme Piñol-Felis ,&nbsp;María-Paz Romero ,&nbsp;Alba Macià ,&nbsp;Laura Rubió-Piqué","doi":"10.1016/j.jchromb.2025.124527","DOIUrl":"10.1016/j.jchromb.2025.124527","url":null,"abstract":"<div><div>A novel method based on volumetric absorptive micro-sampling (VAMS) combined with UPLC-MS/MS was developed and validated to determine the principal (poly)phenolic metabolites in human blood following the consumption of 140 g of purple whole-grain barley (WGB) biscuits. Finger-prick blood samples were collected from 11 healthy volunteers at multiple time points up to 48 h post-ingestion. To extract (poly)phenolic metabolites efficiently, various extraction parameters were optimized. Then, the method was successfully applied and five colonic (poly)phenolic metabolites from the main (poly)phenolic families from barley were detected: benzene-1,2-diol-<em>O</em>-sulphate, 3-(4′-hydroxy-3′-methoxy)propanoic acid and its sulphated form, 5′-(3′,4′-dihydroxyphenyl)-γ-valerolactone-<em>O</em>-sulphate, and methyl luteolin-<em>O</em>-glucuronide. Maximum absorption occurred at 12 h for most metabolites, while luteolin-<em>O</em>-glucuronide showed two distinct peaks at 2 and 6 h, indicating its dual-phase absorption. Comparison with venous plasma samples collected during the 0–6 h period showed no significant differences (<em>p</em> &gt; 0.05), validating the statistical reliability of VAMS as an alternative to venipuncture. Thus, VAMS emerges as a less invasive and statistically robust means for analyzing the pharmacokinetic profile of (poly)phenols, particularly those arising from colonic metabolism.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1256 ","pages":"Article 124527"},"PeriodicalIF":2.8,"publicationDate":"2025-02-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143487927","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Simultaneous analysis of 203 drugs of abuse and metabolites in urine samples using liquid chromatography–tandem mass spectrometry","authors":"Sangeun Lee ,&nbsp;Jihyun Lee ,&nbsp;Dain Jang ,&nbsp;Hee-jung Cho ,&nbsp;Seonmi Choi ,&nbsp;Eunbin Ryu ,&nbsp;Wonhee Koo ,&nbsp;Jaewoo Song ,&nbsp;Jea-sung Pyo ,&nbsp;Na Young Lim ,&nbsp;Chan Hyeok Kwon ,&nbsp;Kikyung Jung ,&nbsp;Jin Young Kim ,&nbsp;Sungill Suh ,&nbsp;Youngmin Hong ,&nbsp;Eunyoung Han","doi":"10.1016/j.jchromb.2025.124524","DOIUrl":"10.1016/j.jchromb.2025.124524","url":null,"abstract":"<div><div>The issue of drug abuse is increasingly becoming a significant concern worldwide. However, the simultaneous detection of a wide spectrum of drug of abuse (DOA), especially in biofluids, is challenging due to their diverse and varied physicochemical properties and matrix effects. Herein, we have developed a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for simultaneous detection of 203 DOAs, including amphetamines, opiates, cathinones, phencyclidines, synthetic cannabinoids, cocaine, and metabolites, in 100 μL of urine. A mass analysis was performed using multiple reaction monitoring mode with an electrospray ionization source. The run time of the developed method was 16 min. Two sample preparation methods were compared for urine samples: enzymatic hydrolysis followed by either dilution or QuEChERS. Both methods demonstrated good linearity and low matrix effects; however, the dilution method showed superior accuracy and precision. Method validation was conducted to assess the efficacy of the developed method. The LC-MS/MS method with the dilution method demonstrated good linearity with the coefficients of determination (R²) above 0.99 for 200 compounds. The limit of quantification (LOQ) ranged from 0.1 to 20.0 ng/mL. The inter-day precision was below 20 % for all 203 compounds, with a bias of ±20 % for 198 compounds. This method was successfully applied to 40 real urine samples. The developed method allows the simultaneous separation and detection of a variety of DOAs with diverse physicochemical properties in a small amount of urine. Furthermore, the technique could be adapted to fit the practical requirements of forensic investigations, thereby enhancing its effectiveness and reliability.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1256 ","pages":"Article 124524"},"PeriodicalIF":2.8,"publicationDate":"2025-02-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143549624","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}