Journal of Chromatography B最新文献

{"title":"Quantitative analysis of three bioactive components of Biancaea decapetala extracts in rat plasma and RAW264.7 cells using UPLC-MS/MS and its application to comparative pharmacokinetics in normal and diseased states","authors":"Yang Zhou ,&nbsp;Pu Wang ,&nbsp;Zuying Zhou ,&nbsp;Meng Zhou ,&nbsp;Mingyan Chi ,&nbsp;Lin Zheng ,&nbsp;Yong Huang","doi":"10.1016/j.jchromb.2024.124356","DOIUrl":"10.1016/j.jchromb.2024.124356","url":null,"abstract":"<div><div><em>Biancaea decapetala</em> (Roth) O.Deg. (Fabaceae), traditionally utilized by the Hmong for treating rheumatoid arthritis (RA), has its pharmacokinetic behavior under disease conditions largely unexplored. In view of this, a UPLC-MS/MS method was established for the determination of protosappanin B (PTB), protosappanin B-3-<em>O-β-D</em>-glucoside (PTD), and 3-deoxysappanchalcone (3-DSC), key bioactive components of the herb, in rat plasma and RAW264.7 cells to explore the effect of disease state on the pharmacokinetic profiles changes of these three components <em>in vitro</em> and <em>in vivo</em>. These components were detected using multiple reaction monitoring (MRM) process in positive and negative mode. Each calibration curve had a high <em>R</em>² value of &gt; 0.99. The intra- and inter-day precisions of PTD, PTB, 3-DSC were all &lt; 15 %, and accuracy ranged from 85 % to 115 %. The RSD values pertaining to stability, recovery, matrix effect, and stability remained below 15.0 %. It was successfully applied for the investigation of the pharmacokinetics of these three components in rat plasma and RAW264.7 cells after administration of <em>Biancaea decapetala</em> extracts (BDE). In rat pharmacokinetic experiments, significant differences were observed in the AUC_(0-t), MRT_(0-t), and <em>Cl</em>_z/<em>F</em> values of PTD, PTB, 3-DSC between adjuvant-induced arthritis (AA) and normal rats. In cellular pharmacokinetic experiments, comparison with the normal group revealed increased AUC_(0-t) and MRT_(0-t) for these three components in the LPS-induced inflammatory cell model, along with decreased <em>Cl</em>_z/<em>F</em>, which was consistent with <em>in vivo</em> experimental outcomes. These findings suggest an increased absorption rate and a decreased elimination rate of the three components of BDE in AA rats and inflammatory cells, indicating a potential alteration in the rate and extent of drug metabolism. This study provided a theoretical reference for further clarification of its pharmacodynamic basis.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1248 ","pages":"Article 124356"},"PeriodicalIF":2.8,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142592621","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":"Quantification of tricyclic glycopeptide in human plasma by UHPLC-MS3 coupled with counter-extraction follow by protein precipitation to enhance sensitivity","authors":"Luyao Yu ,&nbsp;Xiaoqian Chen ,&nbsp;Yingxia Guo ,&nbsp;Jiansong You ,&nbsp;Meiyun Shi ,&nbsp;Yalin Xi ,&nbsp;Lei Yin","doi":"10.1016/j.jchromb.2024.124343","DOIUrl":"10.1016/j.jchromb.2024.124343","url":null,"abstract":"<div><div>An ultra-high performance liquid chromatography tandem mass spectrometry cubed (UHPLC/MS³) assay coupled with protein precipitation and counter-extraction for detection of tricyclic glycopeptide vancomycin in human plasma was established and validated in this study. After protein precipitation and counter-extraction with dichloromethane, chromatographic separation of vancomycin and norvancomycin were performed on a reversed phase column (XBridge Peptide BEH C₁₈ column, 2.1 × 100 mm I.D, 3.5 μm). The transition (parent ions → fragment ions → further fragment ions) at <em>m</em>/<em>z</em> 725.3 → 144.1 → 100.1 was used for quantification of vancomycin. The transition (parent ions → fragment ions) at <em>m</em>/<em>z</em> 718.3 → 144.2 was used for detection of norvancomycin. The linear range of the developed analytical method for quantification of vancomycin was 0.5–100 µg/mL (r = 0.9989). The range of intra- and inter-day precisions of the assay among low, medium and high concentrations is between 1.88 % and 6.33 %. The sensitivity of the analytical method was significantly improved by using MS³ technique as monitoring mode and counter-extraction with dichloromethane followed by protein precipitation as sample processing assay. The developed UHPLC/MS³ assay was successfully applied for clinical therapeutic drug monitoring (TDM) of vancomycin in 45 human plasma samples.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124343"},"PeriodicalIF":2.8,"publicationDate":"2024-10-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142492172","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":"Preparation of attapulgite nanoparticles modified polypropylene adsorption membrane and its application in small molecular pollutant adsorption","authors":"Shuaibin Wu","doi":"10.1016/j.jchromb.2024.124338","DOIUrl":"10.1016/j.jchromb.2024.124338","url":null,"abstract":"<div><div>In this study, a novel surface covalent reaction method was used to modify attapulgite nanoparticles on the surface of polypropylene adsorption membrane to adsorb various small molecular pollutants for the first time. The surface covalent reaction method has the advantage of step control. Therefore, the uniformity and stability of attapulgite nanoparticles can be ensured, and then could effectively improve the adsorption performance of polypropylene adsorption membrane. On the other hand, compared with various materials modified on the surface of polypropylene adsorption membrane currently, attapulgite nanoparticles has the characteristics of low cost and environmental friendliness, which is more conducive to the large-scale practical application. The polypropylene adsorption membrane modified with attapulgite nanoparticles was characterized by field emission scanning electron microscopy, fourier transform infrared spectrometer and X-ray diffractograph, and it was confirmed that the attapulgite nanoparticles was successfully modified on the surface of the polypropylene adsorption membrane. The experimental results showed that the adsorption capacities of polypropylene adsorption membrane modified with attapulgite nanoparticles could reach 11.53 mg/g, 8.7 mg/g and 5.78 mg/g for cyromazine, malachite green and dagenan respectively within 10 s. In the case of the above three analytes, the minimum detected concentration could reach 0.02 mg/mL, and the relative standard deviation was about 10 %. At the same time, the adsorption performance of polypropylene adsorption membrane modified with attapulgite nanoparticles did not decrease significantly after 50 cycles. A standard recovery of 76.8 % − 89.5 % and a relative standard deviation of 7.2 % − 15.2 % were obtained by using the polypropylene adsorption membrane modified with attapulgite nanoparticles to adsorb cyromazine in cucumber skin samples, indicating that the polypropylene adsorption membrane modified with attapulgite nanoparticles has the ability to treat complex samples.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124338"},"PeriodicalIF":2.8,"publicationDate":"2024-10-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142441917","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":"Quantification of Epoxyeicosatrienoic acids Enantiomers: The development of reliable and practical liquid chromatography mass Spectrometry assay","authors":"Fadumo A. Isse ,&nbsp;Sara Helal ,&nbsp;Ahmed A. El-Sherbeni ,&nbsp;Dion R Brocks ,&nbsp;Ayman O.S. El-Kadi","doi":"10.1016/j.jchromb.2024.124346","DOIUrl":"10.1016/j.jchromb.2024.124346","url":null,"abstract":"<div><div>Epoxyeicosatrienoic acids (EETs) are increasingly recognized as key metabolites in the arachidonic acid (AA) metabolic pathway. EETs are epoxy derivatives of AA with two chiral centers formed by cytochrome P450 (CYP) enzymes. EETs have reported biological activities as racemates; however, knowledge on specific optical isomers of EET is lacking. A main reason is the absence of practical assay to quantify EETs isomers associated with specific pathological conditions and enzymes. The reported underivatized chiral LC-MS/MS assays utilize different mobile phases and flow rates or required long run times to achieve separation of EET stereoisomers. Others incorporated a derivatization step before the separation of EETs in their assays. Therefore, the objective of this study was to develop and validate a stereoselective assay for the simultaneous quantitation of underivatized EET enantiomers using Liquid Chromatography Mass Spectrometry (LC-MS/MS) with an optimum baseline separation using binary mobile phase and gradient elution. Herein, we report the development and validation of an LC-MS/MS assay, and its application to quantify the formation of EET enantiomers mediated by human liver microsomes. Assay linearity extends over 10–600 ng/mL with r² &gt; 0.99 for all EETs enantiomers. The inter-run accuracy was within ± 15 %, and precision was ≤ 15 %, and &lt; 20 % for the LLOQ. The matrix effect for the current assay was within ≤ ±20 %, and the mean recovery for quantitative methods was 70–125 %. The assay proved to be reliable and practical for chiral analysis.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124346"},"PeriodicalIF":2.8,"publicationDate":"2024-10-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142492171","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 quantification of polymyxin B in human pulmonary epithelial lining fluid by LC-MS/MS and its clinical application","authors":"Yu Wang ,&nbsp;Xiaofen Liu ,&nbsp;Yan Chen ,&nbsp;Beining Guo ,&nbsp;Jiao Liu ,&nbsp;Jing Zhang","doi":"10.1016/j.jchromb.2024.124332","DOIUrl":"10.1016/j.jchromb.2024.124332","url":null,"abstract":"<div><div>Pulmonary epithelial lining fluid (ELF) was commonly used for the pharmacokinetic study in lower respiratory tract infections. To characterize the intrapulmonary pharmacokinetic properties of polymyxin B following aerosol delivery, we developed and fully validated a liquid chromatography/tandem mass spectrometry (LC/MS/MS) method for quantifying polymyxin B in human bronchoalveolar lavage fluid (BALF). The ELF concentrations were calculated by the BALF values of polymyxin B using urea as a volume normalizer. Chromatographic separation was achieved on a Phonomenex Kinetex XB-C18 column(100 mm × 2.1 mm I.D., 2.6 μm)in acetonitrile and water both containing 0.2 % formic acid. The flow rate was set as 0.4 mL/min for a 3.5 min running time. Protein precipitation was used in preparing BALF samples with polymyxin E1 as an internal standard. Polymyxin B was detected under multiple reaction monitoring conditions using the electrospray ionization interface running in the positive ionization mode. The assay showed a good linear relationship over the tested concentration ranges of 0.0300/0.00306–––10.0/1.02 mg/L for polymyxin B1/B2 in bronchoalveolar lavage fluid (R² &gt; 0.99). The inter- and inter-day precisions (RSD, %) were &lt; 12.2 %(15.2 % for LLOQ samples)and the accuracies (%) were within the range of 94.3 ∼ 110.4 %. This reliable LC–MS/MS method for detection of polymyxin B was successfully applied to conduct a pulmonary penetration study in patients following aerosol administration.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124332"},"PeriodicalIF":2.8,"publicationDate":"2024-10-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142446262","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":"Facile preparation of titanium functionalized cross-linked chitosan polymer for phosphoproteome analysis in serum","authors":"Xiuqin Sheng,&nbsp;Yimin Guo,&nbsp;Chuan-Fan Ding,&nbsp;Yinghua Yan","doi":"10.1016/j.jchromb.2024.124347","DOIUrl":"10.1016/j.jchromb.2024.124347","url":null,"abstract":"<div><div>Efficient phosphopeptide enrichment is extremely important for proteomics research. In this work, chitosan (CTs), 2,3-dihydroxyterephthalaldehyde (2,3-DHA), and carbohydrazide (CHZ) are polymerized to generate the polymer (DHA-CTs-CHZ), and then the polymer (DHA-CTs-CHZ) is coupled with a significant number of titanium ions to enrich phosphopeptides. The material exhibits high selectivity (5000:1 M ratio of BSA to β-casein), sensitivity (0.001 fmol/μL), loading (83.3 μg/mg), recovery (98.6 ± 1.2 %), and effective size exclusion for phosphopeptide enrichment. In addition, 46 phosphopeptides and 31 phosphorylated sites associated with 27 phosphorylated proteins were successfully captured from the serum of normal subjects, while 47 phosphopeptides and 35 phosphorylated sites associated with 30 phosphorylated proteins were successfully captured from Alzheimer’s disease (AD) patients’ serum.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124347"},"PeriodicalIF":2.8,"publicationDate":"2024-10-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142520583","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":"Pharmacokinetic and tissue distribution study of pectolinarigenin in rats using UPLC-MS/MS","authors":"Yingying Pan ,&nbsp;Zihan Tan ,&nbsp;Ping Liu ,&nbsp;Aixia Yang ,&nbsp;Lin-Lin Chen","doi":"10.1016/j.jchromb.2024.124344","DOIUrl":"10.1016/j.jchromb.2024.124344","url":null,"abstract":"<div><div>Pectolinarigenin (PEC), a natural flavonoid isolated from <em>Cirsium japonicum</em>, exhibits promising therapeutic potential for multiple cancers. In present study, a simple and sensitive UPLC-MS/MS method was established for the quantification of PEC in rat plasma and tissues. The assay procedure involved a one-step protein precipitation with tadalafil as the internal standard, and separation on a Welch Xtimate UHPLC C₁₈ column by gradient elution of acetonitrile/aqueous formic acid (0.1 %, v/v) at a flow rate of 0.2 m L·min⁻¹. The detection was conducted using multiple-reaction monitoring via an electrospray ionization source in positive ionization mode. The established method was proved to be highly sensitive with a good linearity (R² &gt; 0.99) in respective concentration range (0.1–100 ng·mL⁻¹ in plasma and 1–10,000 ng·mL⁻¹ in tissues) and acceptable extraction recovery (≥71.17 %), matrix effect and stability, which was applied to study the pharmacokinetics and tissue distribution of PEC after intravenous (100 μg·kg⁻¹) and oral administration (10, 20 and 40 mg·kg⁻¹). PEC was promptly absorbed (<em>T</em>_max ≤ 0.222 h) and maintained at a low level with slow elimination (<em>t</em>_{1/2 z} ≥ 14.47 h) in rats after oral administration, resulting in extremely low bioavailability (0.56–0.68 %). However, PEC is widely distributed in rat tissues with high exposure in GI tract, liver and kidney. The bioavailability and tissue affinity were firstly revealed, which would guide directions for further development of PEC as an anti-tumor drug candidate.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124344"},"PeriodicalIF":2.8,"publicationDate":"2024-10-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142520584","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":"Characterization of etomidate and emerging analogs in human hair using UHPLC-MS/MS and confirmation in real forensic cases","authors":"Lina Pei ,&nbsp;Shuo Yang ,&nbsp;Chaodan Cui ,&nbsp;Xin Wang ,&nbsp;Ping Xiang ,&nbsp;Yonghui Dang ,&nbsp;Yan Shi","doi":"10.1016/j.jchromb.2024.124340","DOIUrl":"10.1016/j.jchromb.2024.124340","url":null,"abstract":"<div><div>The regulation of etomidate, a widely used drug for anesthesia induction and short surgical procedures, has led to the emergence of etomidate analogs such as metomidate, propoxate, and isopropoxate. This study introduces and validates a simple, rapid, and cost-effective ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method for the determination and quantification of etomidate, etomidate acid, metomidate, propoxate, and isopropoxate in human hair. Using a five-minute gradient elution on a Phenomenex Kinetex Biphenyl column, the method achieves low limits of quantification (LOQs), ranging from 5 to 20 pg/mg. Method validation confirms robust linear calibration curves for the target substances in hair samples within the range of LOQs to 1000 pg/mg, with average correlation coefficients (r) all exceeding 0.999. The method also achieves acceptable intra-day and inter-day precision (&lt;15 %) and trueness(bias, −10.9 % to 14.4 %). The matrix effect ranges from 46.9 % to 94.2 %, and the extraction recovery rate ranges from 84.5 % to 105 %. When applied to authentic cases, this method successfully identified 56 positive samples. The concentrations of etomidate, etomidate acid, metomidate, propoxate, and isopropoxate in positive samples ranged from 27 to 1.5 × 10⁵ pg/mg, 21 to 1.5 × 10³ pg/mg, 18 to 8.7 × 10⁴ pg/mg, 25 to 1.6 × 10⁴ pg/mg, and 22 to 5.0 × 10⁵ pg/mg, respectively.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124340"},"PeriodicalIF":2.8,"publicationDate":"2024-10-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142492170","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":"Fe3O4@MXene@PEI aerogel immobilized acetylcholinesterase for inhibitor screening from herbal plants","authors":"Di Zhao ,&nbsp;Zhonghua Li ,&nbsp;Xiaobing Liu ,&nbsp;Zhiyu Zhang ,&nbsp;Huifen Ma ,&nbsp;Pan Wang ,&nbsp;Zhenqiang Zhang ,&nbsp;Junying Song ,&nbsp;Kai Hu","doi":"10.1016/j.jchromb.2024.124345","DOIUrl":"10.1016/j.jchromb.2024.124345","url":null,"abstract":"<div><div>Screening of acetylcholinesterase (AChE) inhibitors is a common strategy in drug discovery for treating Alzheimer’s disease. Herein, AChE was immobilized onto magnetic polyethyleneimine-based MXene aerogels through both electrostatic interactions and covalent bonds, enabling its application in AChE activity assays and inhibitor screening of herbal plants. The composite was analyzed using a range of techniques, including scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), and Zeta potential analysis, to gain insight into its chemical and physical properties. The proposed Fe₃O₄@MXene@PEI<strong>-</strong>AChE composite exhibited enhanced temperature and pH stability, as evaluated by Ellman’s method, along with good reusability. The Michaelis Menten constant (<em>K</em>_m) of the immobilized AChE was calculated to be 0.68 mmol/L. Additionally, an inhibition kinetic study was conducted to verify the feasibility of utilizing the immobilized enzyme to screen for inhibitors, with huperzine A employed as a model inhibitor. The proposed strategy was employed to compare the AChE inhibitory activity of 18 commonly used herbal medicines for treating AD, revealing both the aqueous and alcoholic extracts of Coptis chinensis as exhibiting the highest AChE inhibitory activity. Finally, the screening of AChE inhibitors in Coptis chinensis extracts were conducted by combining the proposed strategy with UPLC-Q-Orbitrap high resolution mass spectrometry. This study presents a feasible strategy for monitoring AChE activity and holds considerable potential for further exploration of AChE-inhibiting active ingredients in herbal medicines.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124345"},"PeriodicalIF":2.8,"publicationDate":"2024-10-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142531351","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":"Quantitative determination by UHPLC-MS/MS of 18 common drugs of abuse and metabolites, including THC and OH-THC, in volumetric dried blood spots: a sustainable method with minimally invasive sampling","authors":"Christina Ververi ,&nbsp;Claudia Gentile ,&nbsp;Marta Massano ,&nbsp;Alberto Salomone ,&nbsp;Marco Vincenti","doi":"10.1016/j.jchromb.2024.124337","DOIUrl":"10.1016/j.jchromb.2024.124337","url":null,"abstract":"<div><div>The increased use of drugs of abuse urges forensic toxicologists to create quick, simple, minimally invasive sampling techniques for biological fluids combined with analytical methods assuring accurate results. To this purpose, a method was developed aimed at quantifying 18 drugs of abuse and metabolites in DBS. Validation of the method was conducted by spiking blank whole blood with the analytes on <em>Capitainer® B</em> cards. The extracts were analyzed by a targeted UHPLC-MS/MS method. Linear calibration was achieved in the range of 1–100 ng/mL for: amphetamine, MDA, MDMA, methamphetamine, cocaine, codeine, benzoylecgonine, cocaethylene, morphine, 6-MAM, buprenorphine, methadone, EDDP, ketamine, norbuprenorphine norketamine, THC, and OH-THC. Experimental LOD was found at 0.5 ng/mL for all analytes except for norbuprenorphine, THC and THC-OH which yielded a LOD of 1 ng/mL. Intra- and inter-day accuracy was satisfactory with bias% resulting within 5%. Evaluation of intra- and inter-day precision yielded CV% values within 20%, for all compounds except EDDP. Average extraction recovery calculated at low (2 ng/mL) and high (75 ng/mL) concentration levels was 63% while average matrix effect determined at the same levels was found to be within 85% − 115% for all analytes except from codeine (70%) and MDMA (131%). The method was applied to authentic blood samples spotted onto the DBS card and the minimum value detected was 1.3 ng/mL. HPLC-MS/MS proved capable to identify all the targeted analytes at low concentrations in the small blood volumes obtainable from DBS cards, which in turn confirmed to be effective and sustainable micro-sampling devices.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124337"},"PeriodicalIF":2.8,"publicationDate":"2024-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142418164","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}