Journal of Chromatography B最新文献

{"title":"Tandem mass tag-based proteomics analysis to reveal growth stage-dependent pathways in Dendrobium nobile Lindl","authors":"Wanhui Chen ,&nbsp;Cong Xie ,&nbsp;Wenying He","doi":"10.1016/j.jchromb.2025.124647","DOIUrl":"10.1016/j.jchromb.2025.124647","url":null,"abstract":"<div><h3>Objective</h3><div>This study aimed to analyze differentially proteins at various growth stages of <em>Dendrobium nobile Lindl</em> and attempt to find some possible functional proteins related to plant growth or pharmacological activity.</div></div><div><h3>Methods</h3><div>The samples were grouped into two categories based on their growth periods as 2–3 years (S1) and 7–8 years (S2), respectively. Tandem Mass Tag(TMT) labeling-based quantitative proteomics combined LC-MS/MS was applied to identify differential protein expression at various growth stages of <em>Dendrobium nobile</em> Lindl<em>.</em> Those proteins were analyzed by various bioinformatics methods. The activities of several antioxidant enzymes including superoxide dismutase(SOD), peroxidase (POD) and catalase (CAT) in the plant were specifically examined using commercially available assay kits.</div></div><div><h3>Results</h3><div>A total of 6032 proteins were identified with 283 differential proteins related to 168 up-regulated and 115 down-regulated. KEGG pathway enrichment analysis revealed that proteins involved in heat shock response, phenylpropanoid biosynthesis, and antioxidant activity showed significant changes across the growth stages. Specifically, a decrease in small heat shock proteins (sHSPs) was observed in older plants, potentially reducing their stress resilience, while proteins involved in lignin biosynthesis, such as SOD, CAT, and POD, were upregulated, suggesting improved stress response.</div></div><div><h3>Conclusion</h3><div>There are 283 differential proteins with diversiform function between different growth stages. Some upregulated antioxidant enzymes contribute to Dendrobium's ability to combat oxidative stress in older plants. These findings provide insights into how protein expression varies with growth stage, offering scientific support for determining optimal harvesting periods or pharmacological mechanism for <em>Dendrobium nobile</em> Lindl<em>.</em></div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1261 ","pages":"Article 124647"},"PeriodicalIF":2.8,"publicationDate":"2025-05-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144084672","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 sulbactam and durlobactam in saline and human plasma via ultra-performance liquid chromatography tandem mass spectrometry","authors":"Hanna F. Roenfanz,&nbsp;David P. Nicolau,&nbsp;Joseph L. Kuti","doi":"10.1016/j.jchromb.2025.124654","DOIUrl":"10.1016/j.jchromb.2025.124654","url":null,"abstract":"<div><div>Sulbactam-durlobactam is a combination β-lactam/β-lactamase inhibitor antibiotic approved in the United States for the treatment of adult patients with hospital-acquired and ventilator-associated bacterial pneumonia due to susceptible isolates of <em>Acinetobacter baumannii-calcoaceticus</em> complex. A liquid chromatography tandem mass spectrometry method for the quantification of sulbactam and durlobactam in human plasma and aqueous matrices has been developed and validated. The standard curves for each drug were linear over the range 0.5 to 50 μg/mL and use the isotopic analogs sulbactam-d₅ and [¹³C₂, ¹⁵N₂]-durlobactam as internal standards for their respective analytes. This simple, reproducible method for the determination of sulbactam and durlobactam concentrations was developed with the intent to conduct future pharmacokinetic analyses and to guide clinical laboratories in the development of a therapeutic drug monitoring assay.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1261 ","pages":"Article 124654"},"PeriodicalIF":2.8,"publicationDate":"2025-05-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144071200","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":"A simple surrogate approach for the quantitation of C4 (7α-hydroxy-4-cholesten-3-one) in human serum via LC-MS/MS and its application in a clinical study","authors":"Feng Yin ,&nbsp;Mani Deepika Vakkalanka ,&nbsp;Walter Wiley ,&nbsp;M. Shane Woolf ,&nbsp;Yousef Basir ,&nbsp;Kumar Shah ,&nbsp;Aaron M. Wheeler ,&nbsp;Moucun Yuan ,&nbsp;William R. Mylott Jr. ,&nbsp;Mike Baratta","doi":"10.1016/j.jchromb.2025.124651","DOIUrl":"10.1016/j.jchromb.2025.124651","url":null,"abstract":"<div><div>We present a validated LC-MS/MS assay for the quantitation of 7α-hydroxy-4-cholesten-3-one (C4), a key intermediate in the bile acid synthesis pathway from cholesterol, in human serum. A surrogate matrix approach was employed to overcome the challenges posed by the endogenous C4 levels in the biological matrix. Human serum samples were spiked with stable isotope labeled internal standard (SIL-IS), processed using supported liquid extraction (SLE), and analyzed by LC-MS/MS. Parallelism was successfully demonstrated between human serum (authentic matrix) and 5 % bovine serum albumin in phosphate buffered saline containing 0.1 % tween 20 (5 % BSA in PBST) (surrogate matrix). The assay's linear analytical range was established from 0.200 to 200 ng/mL. This validated LC-MS/MS method exhibited excellent accuracy and precision. The overall accuracy was between 97.9 % and 101 % with %CV less than 4.0 % for C4 in human serum. C4 was found to be stable in human serum for up to 24.7 h at room temperature, up to 34 days when stored at −25 °C or − 80 °C, and after five freeze/thaw cycles. The assay has been successfully applied to human serum samples to support a clinical study.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1261 ","pages":"Article 124651"},"PeriodicalIF":2.8,"publicationDate":"2025-05-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144071196","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":"A magnetic poly (methacrylic acid-co-ethylene glycol dimethacrylate) copolymer for extraction of anticonvulsants from saliva followed by high performance liquid chromatography analysis","authors":"Camila Gabriela Carrara ,&nbsp;Diailison Teixeira de Carvalho ,&nbsp;Mariana Azevedo Rosa ,&nbsp;Luiz Fernando Gorup ,&nbsp;Maria Betânia de Freitas Marques ,&nbsp;Eduardo Costa Figueiredo","doi":"10.1016/j.jchromb.2025.124635","DOIUrl":"10.1016/j.jchromb.2025.124635","url":null,"abstract":"<div><div>Neurological diseases like epilepsy are commonly treated with anticonvulsants, and the dosage control of these medications has been carried out with therapeutic biomonitoring, mainly in blood. Saliva is a less invasive sample, and its drug concentration is proportional to the blood fraction concentration not bound to the proteins, making it an important alternative to blood. Therefore, this study describes the synthesis of a magnetic poly (methacrylic acid-<em>co</em>-ethylene glycol dimethacrylate) copolymer (M-CP) and its use in magnetic dispersive solid phase extraction of primidone (PMR), phenobarbital (PB), phenytoin (PHT), and carbamazepine (CB) from saliva, followed by their determination by high performance liquid-chromatography. M-CP was synthesized in 4 steps and the material was characterized by infrared spectroscopy, scanning electron microscopy, zeta potential, and thermal analysis. The sample preparation protocol was optimized by central composite rotatable design and the optimal conditions were obtained for pH 5.78, 12.8 mg of M-CP, and 2.18 mL of diluted saliva. In the adsorption studies, the Avrami and Jovanovic models demonstrated the best fit for describing the adsorption kinetics and isotherm, respectively. The equilibrium time was reached in 60 min, and 10.96 mg g⁻¹ was the maximum adsorption capacity. The developed method was linear (R² &gt; 0.99) in the range of 2 to 30 mg L⁻¹ for PMR and PB, 1 to 20 mg L⁻¹ for PHT, and 1 to 30 mg L⁻¹ for CBZ. Precisions were obtained in the range of 1.35 to 19.44 %, and accuracy from −14.92 % to 18.83 %. The limits of detection ranged from 0.48 to 1.30 mg L⁻¹, while the limits of quantification were lower than the therapeutic levels of each drug, being suitable for the method application. The developed method is simple, fast, and requires few amounts of saliva, sorbent, and solvents, being a good alternative for the therapeutic biomonitoring of anticonvulsants in saliva samples.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1261 ","pages":"Article 124635"},"PeriodicalIF":2.8,"publicationDate":"2025-05-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144071199","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":"Determination of tacrolimus in whole blood of pediatric liver transplant patients by UPLC–MS/MS: Informed its individualized dose","authors":"Saisai Ling ,&nbsp;Ying Jin ,&nbsp;Cuiyao He ,&nbsp;Lisha Fu ,&nbsp;Yuhua Deng ,&nbsp;Xiaohui Qi ,&nbsp;Zhenglei Wang ,&nbsp;Yiying Wu","doi":"10.1016/j.jchromb.2025.124645","DOIUrl":"10.1016/j.jchromb.2025.124645","url":null,"abstract":"<div><div>Tacrolimus is a potent macrolide immunosuppressant widely used in pediatric liver transplant patients. However, its narrow therapeutic window and significant inter-individual pharmacokinetic differences result in a poor correlation between blood concentrations and administered doses. To support its individualized dose, a sensitive, fast and robust ultra-high performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method was developed to measure tacrolimus concentrations in whole blood of pediatric liver transplant patients. The method employed acetonitrile for protein precipitation, and sample separation was achieved using an Acquity UPLC CSH C₁₈ column (2.1 × 50 mm, 1.7 μm) with gradient elution. The mobile phase consisted of ammonium solution–water (0.5:1000, <em>v</em>/v) and methanol. The method demonstrated good linearity within a concentration range of 0.20–50.00 ng/mL. The intra- and inter-day precisions of tacrolimus in whole blood were less than 13.5 %, with the accuracy ranged from −7.2 % to 13.0 %. Selectivity, carryover, matrix effects, recovery, dilution reliability, and stability all met the standards set by relevant guidelines. The established UPLC–MS/MS method was successfully applied to measure the concentration of tacrolimus in the whole blood of pediatric liver transplant patients and support its individualized dose. Under the rapid UPLC–MS/MS method, 25 (65.8 %) patients required a dose increase, 3 (7.9 %) patients needed a dose reduction, and 10 (26.3 %) patients maintained their original dosage without adjustment.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1261 ","pages":"Article 124645"},"PeriodicalIF":2.8,"publicationDate":"2025-05-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143935284","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":"High-performance liquid chromatography strategy for purifying the transmembrane band 3 protein","authors":"Aline Marzano-Miranda ,&nbsp;Jamil S. Oliveira ,&nbsp;Marla P.C. Marcelino ,&nbsp;Adalberto A. Pereira-Filho ,&nbsp;João Victor N. Starlino ,&nbsp;Gilmar R.F. Pascoal ,&nbsp;Daniella C. Bartholomeu ,&nbsp;Vanessa G. Fraga ,&nbsp;Erika M. Braga","doi":"10.1016/j.jchromb.2025.124631","DOIUrl":"10.1016/j.jchromb.2025.124631","url":null,"abstract":"<div><div>Band 3 is the most abundant protein in the red blood cell membrane and has garnered increasing attention across various research fields. However, commercially available recombinant Band 3 is limited to its cytoplasmic domain, typically produced in <em>Escherichia coli</em>, rendering it unsuitable for studies involving the transmembrane region. Furthermore, the purification of Band 3 from red blood cells (RBC) presents challenges due to its strong interactions with membrane and cytoskeletal proteins, often necessitating immunoprecipitation as the primary method to obtain it in a soluble form. This study validates a chromatographic strategy for purifying Band 3 from erythrocyte membranes. Soluble ghosts were processed using reverse-phase chromatography followed by size-exclusion chromatography. Molecular weight validation was performed using polyacrylamide gels, and the presence of soluble Band 3 was confirmed through western blot analysis. This method leverages the physicochemical properties of proteins—specifically their hydrophobicity and size—to facilitate the cost-effective and efficient purification of Band 3.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1261 ","pages":"Article 124631"},"PeriodicalIF":2.8,"publicationDate":"2025-05-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143935285","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":"Investigations on human biomonitoring for assessing the exposure to synthetic rose oxide in the general population","authors":"Carmen Tiwald ,&nbsp;Veronika Spindler ,&nbsp;Max Scherer ,&nbsp;Nikola Pluym ,&nbsp;Oliver Peschel ,&nbsp;Edgar Leibold ,&nbsp;Gerhard Scherer","doi":"10.1016/j.jchromb.2025.124629","DOIUrl":"10.1016/j.jchromb.2025.124629","url":null,"abstract":"<div><div>Rose oxide (RO) is used in cosmetic, hygiene, laundry, cleaning, and household products as a synthetic fragrance. Synthetic rose oxide differs from naturally occurring rose oxide in its enantiomer composition. While natural RO consists mainly of the (−)-cis isomer, synthetic RO contains approximately equal parts of (−)-cis and (+)-cis isomers, as well as small amounts of (−)-trans and (+)-trans isomers. Since in this project, the exposure to industrially produced chemicals by human biomonitoring (HBM) was in the focus, the method development aimed at suitable urinary metabolites derived from the (+)-cis isomer of synthetic RO. For the identification of biomarkers of exposure to synthetic RO as well as for assessing its toxicokinetics, 5 subjects were administered a single oral (0.1 mg/kg body weight) and dermal (0.5 mg/kg) dose of synthetic RO. Analysis of urine fractions by means of high-resolution mass spectrometry (HRMS, conducted with an Orbitrap instrument) revealed that 9-hydroxy-RO (9-OH-RO), 2-hydroxy-4-carboxy-RO (HC-RO), and di-hydroxy-RO and a lactone derived from ring-hydroxylated RO were potential biomarkers of exposure to synthetic RO. Unfortunately, attempts to develop and validate a HBM method for one of these metabolites failed due to insufficient sensitivity (9-OH-RO) or unavailability of standard materials for the required enantiomers (HC-RO, di-OH-RO), lactone). Alternatively, a headspace-solid-phase-micro-extraction-GC–MS (HS-SPME-GC–MS) method for the parent compound (+)-cis-RO was developed and validated. DVB (divinyl benzene)/PDMS (polydimethylsiloxane) fibers suited best for the extraction. Enantiomeric separation was achieved on a Lipodex G column with a temperature gradient. (+)-cis-RO was detected in electron impact ionization (EI) mode. The method performed well with a lower limit of quantification (LLOQ) of 1 ng/L, precision of &lt;10 % and accuracy of &gt;90 %. After oral application, urinary excretion of (+)-cis-RO was fast (mean half-life: 4.1 h) and almost complete after 48 h. However, the mean urinary excretion rate in the 5 subjects amounted to only 7 ppm. (+)-cis-RO was found to be at or slightly above the LLOQ in about half of 14 urine samples from the general population.</div><div>In conclusion, our investigations for the first time provide data for RO metabolism and toxicokinetics in humans. Despite good to excellent performance, the newly developed and validated HS-SPME-GC–MS method for (+)-cis-RO in urine is only of limited value for HBM of exposure to synthetic RO in the general population, due to the tiny urinary excretion rate of unmetabolized RO and the potential risk of contamination with environmental RO during urine collection and subsequent analytical steps. For a suitable HBM method, potential RO metabolites would need to be synthesized in enantiomerically pure form. Our study provides possible candidates for this approach.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1260 ","pages":"Article 124629"},"PeriodicalIF":2.8,"publicationDate":"2025-05-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143918229","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":"Supermacroporous cryogel membranes via polyethyleneimine-assisted decoration for efficient removal of bacterial endotoxin","authors":"Alper Akın ,&nbsp;Semra Akgönüllü ,&nbsp;Duygu Çimen ,&nbsp;Adil Denizli ,&nbsp;Handan Yavuz","doi":"10.1016/j.jchromb.2025.124636","DOIUrl":"10.1016/j.jchromb.2025.124636","url":null,"abstract":"<div><div>The endotoxin, which is a highly pathogenic toxin released from the cell wall of gram-negative bacteria after death, can lead to critical diseases such as sepsis and intestinal inflammation. Poly 2-hydroxyethyl methacrylate (HEMA)-glycidyl methacrylate (GMA)/polyethyleneimine (PEI) cryogel membranes employed for endotoxin removal were synthesized via the immobilization of PEI solution with poly(HEMA-GMA) membranes. The concentration of the treated PEI% solution, the concentration of the endotoxin solution, and the ambient temperature influenced the endotoxin binding percentage of poly(HEMA-GMA) cryogel membranes. Maximum endotoxin removal was observed with poly(HEMA-GMA) cryogel membranes treated with a 25 % PEI solution at 25 °C. Additionally, it was noted that poly(HEMA-GMA)/PEI cryogel membranes exhibited increased endotoxin binding with rising endotoxin concentrations. The percentage of endotoxin bound by cryogel membranes in both aqueous solutions and artificial plasma media increases with the endotoxin concentration in the solutions. The Limulus Amebocyte Lysate (LAL) assay results show that the percentages of bound endotoxin in artificial plasma and aqueous solutions are approximately equivalent. The prepared poly(HEMA-GMA)/PEI adsorbent exhibited good reusability and offered high removal ability for endotoxin. The adsorption process can be accurately described by Langmuir adsorption isotherm model.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1261 ","pages":"Article 124636"},"PeriodicalIF":2.8,"publicationDate":"2025-05-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143935286","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":"Machine learning and chemometric methods for high-throughput authentication of 53 Root and Rhizome Chinese Herbal using ATR-FTIR fingerprints","authors":"Xiaoyu Liu ,&nbsp;Xiaokang Liu ,&nbsp;Jiawei Wang ,&nbsp;Daidi Zang ,&nbsp;Yang Yang ,&nbsp;Qinhua Chen ,&nbsp;De-an Guo","doi":"10.1016/j.jchromb.2025.124630","DOIUrl":"10.1016/j.jchromb.2025.124630","url":null,"abstract":"<div><div>To address the identification challenges caused by morphological similarities in Root and Rhizome Chinese Herbal (RRCH), this study developed a discrimination system integrating Attenuated Total Reflectance Fourier Transform Infrared Spectroscopy (ATR-FTIR) with multimodal machine learning. 53 kinds of RRCH collected from China were analyzed using ATR-FTIR to acquire spectral fingerprints. An innovative analytical framework was established, combining chemometric Partial Least Squares Discriminant Analysis (PLS-DA) with optimized machine learning models: t-distributed Stochastic Neighbor Embedding (t-SNE), optimized decision trees, optimized discriminant analysis, naive Bayes, optimized SVM, optimized KNN, SVM kernels, and optimized ensemble learning. Multivariate analysis revealed distinct spatial distribution patterns of chemical characteristics among the 53 RRCH species. t-SNE projections demonstrated significant cluster separation in two-dimensional feature space, confirming strong correlations between spectral fingerprints and phytochemical compositions. The SVM model outperformed others, achieving 100 % classification accuracy on both training and validation sets, with a markedly shorter identification time compared to PLS-DA. This ATR-FTIR-machine learning hybrid system enables high-throughput authentication of RRCH and establishes a scalable technical framework for herbal quality standardization. The methodology provides critical insights into chemical marker discovery through vibrational spectrum-feature relationship mapping, advancing intelligent discrimination of botanically similar medicinal materials.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1260 ","pages":"Article 124630"},"PeriodicalIF":2.8,"publicationDate":"2025-05-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143903934","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":"Detection of flunixin meglumine in pork based on magnetic solid-phase extraction technology","authors":"Kai-yue Qin ,&nbsp;Li He ,&nbsp;Yun-peng Feng ,&nbsp;Xiao-xin Hu ,&nbsp;Ting-yu Xu ,&nbsp;Ying Dong ,&nbsp;Zhen-jun Jia","doi":"10.1016/j.jchromb.2025.124633","DOIUrl":"10.1016/j.jchromb.2025.124633","url":null,"abstract":"<div><div>This study established two methods for detecting flunixin meglumine (FM) in pork. The MSPE-LC-MS/MS method utilizes the accuracy and quantifiability of liquid chromatography-tandem mass spectrometry. FM in pork can be accurately analyzed after optimizing the pretreatment, liquid phase conditions, and mass spectrometry parameters. It shows a good linear relationship (correlation coefficient &gt; 0.999), with a detection limit of 0.2 μg/kg, limit of quantification of 0.6 μg/kg, spiked recovery rates of 90.6 % - 97.4 %, matrix effects of 96.7 % - 107.2 %, intra-day precision of 1.4 % - 5.6 %, and inter-day precision of 4.3 % - 11.5 %. The RP-MSPE-CGIA method combines the separation performance of reversed magnetic solid-phase extraction and the rapidness of colloidal gold immunochromatography. By optimizing conditions, it successfully extends the dairy product detection method to pork. It is easy to operate, has a detection limit of 5 μg/kg, and detection time less than half of MSPE - LC-MS/MS. Experiments show that the two methods complement each other in advantages and can meet the detection requirements of FM in pork in different scenarios.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1260 ","pages":"Article 124633"},"PeriodicalIF":2.8,"publicationDate":"2025-05-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143928588","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}