Mo Wang, Shun-Li Zhang, Rui Zhang, Yi-Chuan Song, Jie Shi, Qiao-Zhen Xue, Yan-Wei Hu
{"title":"[Establishment and international comparison of reference methods for glycated hemoglobin].","authors":"Mo Wang, Shun-Li Zhang, Rui Zhang, Yi-Chuan Song, Jie Shi, Qiao-Zhen Xue, Yan-Wei Hu","doi":"10.3724/SP.J.1123.2025.03017","DOIUrl":"10.3724/SP.J.1123.2025.03017","url":null,"abstract":"<p><p>To promote the standardization and harmonization of glycated hemoglobin A1c (HbA1c) testing results in medical laboratories across Beijing, we established a reference method for HbA1c. This method participated in the International Comparison Program for HbA1c Reference Laboratories organized by the European Reference Laboratory Network for HbA1c to validate its accuracy. The experimental samples consisted of HbA1c network reference laboratory proficiency testing samples imported annually from the Netherlands, including six calibrators (A-F), ten intercomparison samples, several quality control materials, and additional auxiliary samples with International Federation of Clinical Chemistry and Laboratory Medicine (IFCC)-assigned values. The pre-treatment process involved digesting samples with protein endopeptidase Glu-C. The experimental samples were removed from the -80 ℃ freezer and allowed to reach room temperature. Subsequently, 50 μL of Glu-C (mass concentration: 200 μg/mL) was added to each sample vial at a ratio of total hemoglobin to enzyme of 1 mg∶0.01 mg. The volume was then adjusted to a final volume of 500 μL with ammonium acetate solution (50 mmol/L, pH 4.3). After thorough mixing, the samples were incubated at 37 ℃ for 18-20 h. Using mobile phases of methanol and 0.1% formic acid aqueous solution under gradient elution conditions, the detection of HbA1c in international samples was performed via high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). A gradient elution mode was employed for liquid chromatography separation using a Shimadzu C18 column (50 mm×3 mm, 2.2 μm). The injector temperature was maintained at 4-8 ℃, with a column temperature of 30 ℃. The flow rate was kept constant at 0.6 mL/min, with an injection volume of 5 μL and a total run time of 8 min. The MS detection was performed using electrospray ionization (ESI) in positive ion mode with multiple reaction monitoring (MRM). The monitored ion pairs for the precursor and product ions of non-glycated and glycated N-terminal hexapeptides are <i>m/z</i> 348.2/237.2 and <i>m/z</i> 429.2/245.2, respectively. The linearity was evaluated by performing regression analysis. The HbA1c (mmol/mol) quantification in unknown samples was achieved by performing linear regression using Analyst 1.6.2 software. Peak areas were integrated, with the abscissa (X-axis) representing the known concentration ratio of HbA1c to hemoglobin A0 (HbA0), and the ordinate (Y-axis) representing the average peak area ratio of glycated to non-glycated hexapeptides. Both glycated and non-glycated hexapeptides eluted within 3 min, with linear correlation coefficients ranging from 0.999 6 to 0.999 8. The quality control (QC) materials (≥3 types) annually provided by the IFCC were analyzed. Since each QC material in every shipment typically consists of two replicated vials, enzymatic digestion was performed in two separate batches. For each batch, five parallel samples were process","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 3","pages":"248-256"},"PeriodicalIF":0.0,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12980504/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147439070","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}
{"title":"[Rapid determination of venetoclax in plasma by ultra performance liquid chromatography-tandem mass spectrometry].","authors":"Ying Zhu, Xiao-Li Ma, Song-Lin Yu, Ling Qiu","doi":"10.3724/SP.J.1123.2025.06002","DOIUrl":"10.3724/SP.J.1123.2025.06002","url":null,"abstract":"<p><p>Leukemia is a malignant tumor of the hematological system characterized by the uncontrolled proliferation of abnormal hematopoietic cells in the bone marrow. It often presents with anemia, bleeding tendency, infection risk and organ invasion. These clinical symptoms bring severe survival risks to patients. Although traditional chemotherapy regimens are effective in the treatment of some hematological malignancies, their efficacy is limited for elderly patients, those with high-risk genetic characteristics or comorbidities. In recent years, targeted drugs have revolutionized the treatment of leukemia. By selectively inducing tumor cell apoptosis, they have significantly improved the remission rate and survival prognosis of patients with multiple leukemia subtypes. Venetoclax is a B-cell lymphoma 2 (BCL-2) inhibitor and plays an important role in the clinical treatment of hematological malignancies, such as acute myeloid leukemia and chronic lymphocytic leukemia. In addition, it also shows potential efficacy in other hematological malignancies such as multiple myeloma and mantle cell lymphoma. Although the efficacy of venetoclax is remarkable, the individual differences in blood drug concentration are significant due to factors such as drug interactions, polymorphisms of metabolic enzymes, and liver and kidney function. Venetoclax exhibits significant inter-individual pharmacokinetic differences, the trough concentration is significantly correlated with the treatment response, and if the peak concentration exceeds the warning concentration, adverse reactions will be triggered. Clinical trials have reported a variety of adverse events associated with venetoclax, including neutropenia, tumor lysis syndrome, thrombocytopenia, infection, anemia, diarrhea, nausea, upper respiratory tract infection, cough and musculoskeletal pain. Therefore, to minimize the risk of adverse events in the clinical use of venetoclax as much as possible, it is necessary to reasonably guide its clinical dosage. Therapeutic drug monitoring can optimize individual dosing regimens by measuring the steady-state concentration in patients' blood. This research aims to establish a rapid, sensitive and reliable ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method. This method is used for the quantitative determination of venetoclax in plasma, and its performance was validated. This method employs an electrospray ionization and multiple reaction monitoring (MRM) in the positive ion mode to detect venetoclax and its isotope internal standard venetoclax-d<sub>8</sub>. Methanol was used for protein precipitation, C18 reversed-phase chromatographic column was used for liquid phase separation. Gradient elution was performed using acetonitrile and 0.1% formic acid aqueous solution as the mobile phases. The flow rate was 0.4 mL/min, the run time was 3.5 min, and the retention time of venetoclax was 1.95 min. The analysis time is short, facilitationg the ","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 3","pages":"357-362"},"PeriodicalIF":0.0,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12980510/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147438614","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}
{"title":"[Analysis of stimulating factors for serum copeptin based on liquid chromatography-tandem mass spectrometry].","authors":"Dan-Ni Mu, Zhi-Hong Qi, Yi-Chen Ma, Yu-Meng Gao, Yue-Meng Li, Qi Zhang, Song-Lin Yu, Ling Qiu, Xin-Qi Cheng","doi":"10.3724/SP.J.1123.2025.05010","DOIUrl":"10.3724/SP.J.1123.2025.05010","url":null,"abstract":"<p><p>Copeptin, as a stable surrogate biomarker for arginine vasopressin (AVP), plays an important role in the differential diagnosis of polyuria-polydipsia syndromes. Current guidelines recommend dynamic monitoring of copeptin levels during stimulation tests to assist in differentiating AVP deficiency (AVP-D) from primary polydipsia. Although these methods are well-established, they have certain limitations. Therefore, safer and more feasible stimulants with reliable effects are of clinical interest. Additionally, the currently available copeptin assay, which is based on time-resolved immunofluorescence assay, can be subject to interference from autoantibodies or hemolysis. This study aims to evaluate the effects of four common stimulants used in growth hormone function tests, namely levodopa, insulin, glucagon, and octreotide, on copeptin levels using a reliable liquid chromatography-tandem mass spectrometry (LC-MS/MS) method developed in our laboratory. A total of 62 subjects undergoing growth hormone function tests were retrospectively enrolled and stratified by stimulation type: levodopa (<i>n</i>=28), insulin-induced hypoglycemia (<i>n</i>=7), glucagon (<i>n</i>=20), and octreotide (<i>n</i>=7). Blood samples were collected at baseline, 30, 60, 90, and 120 min (for the glucagon stimulation test, samples were collected at 120 and 180 min) for growth hormone determination. Copeptin levels at each time point were measured using LC-MS/MS. The effects of stimulation and correlations were analyzed using the Wilcoxon paired signed-rank test, Mann-Whitney test, and Spearman correlation analysis. The results demonstrated that copeptin levels increased under levodopa stimulation by a maximum of 8.47-fold of baseline (<i>p</i><0.000 1), under insulin stimulation by a maximum of 5.85-fold of baseline (<i>p</i>=0.031 2), under glucagon stimulation by a maximum of 1.43-fold of baseline (<i>p</i><0.000 1), and decreased under octreotide to 43% of baseline (<i>p</i><0.05). No significant correlation was observed between copeptin level changes and those in growth hormone levels. In the levodopa-stimulation group, the maximum value of copeptin in patients with AVP deficiency was significantly lower than that in non-AVP deficiency patients (<i>p</i>=0.000 2), and the area under the receiver operating characteristic curve was 0.98 (95% confidence interval 0.94-1.00, <i>p</i>=0.002 1). Our results demonstrate that levodopa and insulin can effectively stimulate copeptin secretion, whereas octreotide exhibits a suppressive effect. These findings offer important physiological insights into AVP regulation and indicate that certain GH stimulation agents may have extended utility in copeptin-based diagnostic strategies. The LC-MS/MS method for detecting copeptin has potential clinical value in the diagnosis of patients with AVP deficiency and can provide a new detection method for clinical practice. However, the relatively small sample sizes restrict the statistical ","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 3","pages":"302-311"},"PeriodicalIF":0.0,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12980517/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147439012","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}
{"title":"[Preface for Special Issue on Clinical Analysis].","authors":"Si-Ming Wang, Jing-Wu Kang","doi":"10.3724/SP.J.1123.2026.01008","DOIUrl":"10.3724/SP.J.1123.2026.01008","url":null,"abstract":"","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 3","pages":"225"},"PeriodicalIF":0.0,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12980506/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147439053","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}
{"title":"[Lipid metabolomics-based biomarker analysis of neonatal sepsis in serum and cerebrospinal fluid].","authors":"Wei-Xiang Wu, Fu-Qiang Diao, Jun-Fei Guo, Chun-Ming Gu, Li-Hong Wu, Ming-Yong Luo","doi":"10.3724/SP.J.1123.2025.06003","DOIUrl":"10.3724/SP.J.1123.2025.06003","url":null,"abstract":"<p><p>Neonatal sepsis remains a leading cause of morbidity and mortality among newborns worldwide. Despite advances in neonatal care, early diagnosis of sepsis remains challenging due to the lack of sensitive and specific biomarkers. While serum-based indicators have been widely studied, lipid metabolism in cerebrospinal fluid (CSF) remains relatively underexplored, limiting our understanding of central nervous system involvement (CNS) in the early stages of neonatal sepsis. This study aimed to systematically investigate lipid metabolic alterations in both serum and CSF samples from neonates with confirmed sepsis and to identify potential lipid biomarkers for early diagnosis. Seventeen neonates with blood culture-positive sepsis and seventeen controls with negative blood culture results were enrolled from the Neonatal Intensive Care Unit of Guangdong Women and Children Hospital (Women and Children's Hospital, Southern University of Science and Technology) between February 2020 and August 2023. Paired serum and CSF samples were collected and analyzed using targeted lipidomics based on liquid chromatography-tandem mass spectrometry (LC-MS/MS). Univariate analyses, including Student's <i>t</i>-tests and Mann-Whitney U tests, were applied to identify statistically significant differences in lipid levels between groups. Multivariate analyses, including principal component analysis (PCA) and orthogonal partial least squares discriminant analysis (OPLS-DA), were employed to further evaluate group separation and identify discriminatory lipid species. Pathway enrichment analysis was performed using the Kyoto Encyclopedia of Genes and Genomes (KEGG) database, and candidate biomarkers were selected using the Boruta feature selection algorithm and evaluated for diagnostic performance using receiver operating characteristic (ROC) curve analysis. A total of 322 lipid metabolites were identified in serum, with cholesteryl esters (CE), triacylglycerols (TAG), and phosphatidylcholines (PC) being the most abundant lipid classes. In the sepsis group, levels of nearly all lipid subclasses were significantly decreased compared to controls (<i>P</i><0.05), except for TAG and diacylglycerols (DAG), which were not significantly altered. In CSF, 300 lipid species were detected, dominated by CE, PC, and phosphatidylethanolamines (PE). Significantly reduced levels of PE, ceramides (Cer), and lyso phosphatidylethanolamines (LPE) were observed in septic neonates (<i>P</i><0.05). PCA plots demonstrated tight clustering of quality control (QC) samples, indicating high analytical reproducibility and stable instrument performance. In serum, PCA accounted for 66.1% of total variance, showing preliminary group separation that was further confirmed by OPLS-DA (<i>R</i>²<i>Y</i>=0.601, <i>Q</i>²<i>Y</i>=0.271), which identified 107 significantly downregulated lipid metabolites. Similarly, CSF PCA explained 75.7% of the variance, and OPLS-DA (<i>R</i>²<i>Y</i>=0.579, <i>Q</i>²<i>Y</i","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 3","pages":"286-295"},"PeriodicalIF":0.0,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12980514/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147439072","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}
{"title":"[Preparation of magnetic bifunctional materials for exosome capture from serum and phosphopeptide enrichment].","authors":"Zi-Rui Wang, Hai-Jiao Zheng, Qiong Jia","doi":"10.3724/SP.J.1123.2025.04034","DOIUrl":"10.3724/SP.J.1123.2025.04034","url":null,"abstract":"<p><p>As a clinical sample, serum is widely used in disease research due to the minimally invasive nature of its collection and easy accessibility. Exosomes in serum not only carry various bioactive substances such as proteins and nucleic acids but also participate in intercellular communication, which is closely associated with the development of multiple diseases. As one of the most critical post-translational modifications, protein phosphorylation dynamically regulates cellular signaling networks and participates in disease pathogenesis. However, due to the low abundance of exosomes in serum and the fact that phosphoproteins constitute only 1%-2% of the total proteome, direct analysis of exosomal phosphoproteins from serum faces significant challenges. The specific expression of phosphoproteins in exosomes provides novel perspectives for disease diagnosis. In this study, magnetic bifunctional nanoparticles (MagphTi<sup>4+</sup>) based on 2-trifluoromethyl-4-aminobenzoic acid and Ti<sup>4+</sup> were synthesized, which anchor the exosome bilayer membrane through the hydrophobic interactions of 2-trifluoromethyl-4-aminobenzoic acid and the electrostatic interactions of Ti<sup>4+</sup>, and the magnetic responsiveness ensures the isolation of exosomes. Simultaneously, the enrichment of phosphopeptides was achieved by the chelation between Ti<sup>4+</sup> and phosphate groups. MagphTi<sup>4+</sup> was characterized by cold field scanning electron microscopy, thermogravimetric analysis, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy and zeta potential measurement, demonstrating the successful synthesis and functional characteristics of MagphTi<sup>4+</sup>. The precise recognition and rapid separation of exosomes were validated by cold field scanning electron microscopy, transmission electron microscopy and sodium dodecyl sulfate-polyacrylamide gel electrophoresis. Using <i>β</i>-casein as a standard phosphoprotein model, a magnetic solid-phase extraction (MSPE)-matrix-assisted laser desorption ionization-time of flight mass spectrometry platform was established, which demonstrated high selectivity (mass ratio of <i>β</i>-casein to bovine serum albumin was 1∶5 000) and sensitivity (detection limit was 0.4 fmol/μL) for phosphopeptide detection. Subsequently, the method was applied to saliva and nonfat milk samples; 11 phosphopeptides were identified in saliva and 20 were identified in nonfat milk, which demonstrates excellent enrichment capability for phosphopeptide detection in real samples. When applied to clinical serum samples, the method successfully achieved the extraction of exosomes in serum and enrichment of phosphopeptides with low abundance. This integrated approach provides a powerful tool for exosome capture and phosphopeptide enrichment from complex biological samples, showing significant potential for high-throughput phosphoproteomic analysis of exosomes from clinical serum and the screening of disease bioma","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 3","pages":"338-348"},"PeriodicalIF":0.0,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12980519/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147438537","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}
Bao-Bin Luo, Jing-Ran Jiao, Jing Bai, Xiang-Yi Liu
{"title":"[Determination of vitamin A and vitamin E in human tear by liquid chromatography-tandem mass spectrometry and analysis of their relationship with dry eye].","authors":"Bao-Bin Luo, Jing-Ran Jiao, Jing Bai, Xiang-Yi Liu","doi":"10.3724/SP.J.1123.2025.06017","DOIUrl":"10.3724/SP.J.1123.2025.06017","url":null,"abstract":"<p><p>Dry eye is characterized as a multifactorial disorder affecting the tear film and ocular surface, leading to symptoms of discomfort and visual disturbances, with the potential for ocular surface damage. It is among the most prevalent ocular surface disorders, with an estimated prevalence ranging from 5.0% to 50.0%, and an overall prevalence between 21.0% and 50.4% in China. Despite its high global prevalence, the fundamental mechanisms underlying the pathology of dry eye remain largely unexplored. Vitamins are crucial for maintaining ocular surface homeostasis, with vitamins A and E being physiologically present and essential for cell differentiation, development, and proper function. Deficiencies in these vitamins are frequently associated with dry eye, and systemic supplementation has been shown to benefit patients with low vitamin intake. Vitamins A and E may have potential clinical predictive value for the diagnosis and treatment of dry eye. In this study, a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed to simultaneously measure the concentrations of vitamins A and E in human tears. A Phenomenex Kinetex C18 column was employed for gradient elution at a flow rate of 0.4 mL/min. The mobile phase A consisted of a 0.1% formic acid aqueous solution, while mobile phase B comprised a 2 mmol/L ammonium acetate and 0.1% formic acid methanol solution. Positive atmospheric pressure chemical ionization in multiple reaction monitoring mode was utilized for MS/MS detection. The analytical method for vitamin A demonstrated a validated linear range of 5.00-300.00 ng/mL, with a limit of detection at 2.00 ng/mL. The spiked recoveries were between 98.3% and 104.7%, and intra- and inter-day precision ranged from 1.2% to 7.0%. Similarly, the method for vitamin E exhibited a validated linear range of 25.00-1 000.00 ng/mL, with a limit of detection at 6.00 ng/mL. The spiked recoveries ranged from 97.9% to 105.5%, and intra- and inter-day precision varied between 3.0% and 5.7%. Tear samples from five patients with dry eye and nine healthy volunteers were analyzed using this method. In the dry eye group, the average concentrations of vitamin A and vitamin E were 9.60 (5.13-12.54) ng/mL and 42.00 (31.75-128.00) ng/mL, respectively. In the healthy group, the average concentrations of vitamin A and vitamin E were 18.10 (12.46-21.69) ng/mL and 211.00 (181.00-459.75) ng/mL, respectively. Statistical differences in vitamin A and vitamin E levels between the dry eye group and the healthy group were identified using the Wilcoxon Mann-Whitney test (<i>P</i><0.05). This study introduces a straightforward and reliable LC-MS/MS method for the detection of tear VA and VE levels, while also investigating their association with dry eye. This offers a novel reference for understanding the potential risk factors associated with dry eye.</p>","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 3","pages":"296-301"},"PeriodicalIF":0.0,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12980511/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147439037","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}
Jie Shi, Mo Wang, Qiao-Zhen Xue, Shun-Li Zhang, Yan-Wei Hu
{"title":"[Teaching practice of undergraduate graduation projects in clinical laboratory science integrating liquid chromatography-tandem mass spectrometry and external quality assessment].","authors":"Jie Shi, Mo Wang, Qiao-Zhen Xue, Shun-Li Zhang, Yan-Wei Hu","doi":"10.3724/SP.J.1123.2025.06030","DOIUrl":"10.3724/SP.J.1123.2025.06030","url":null,"abstract":"<p><p>This study aimed to explore the application and pedagogical innovation of liquid chromatography-tandem mass spectrometry (LC-MS/MS) in undergraduate thesis training for medical laboratory science students. Using the development of 25-hydroxyvitamin D<sub>2</sub> (25(OH)D<sub>2</sub>) and 25-hydroxyvitamin D<sub>3</sub> (25(OH)D<sub>3</sub>) external quality assessment (EQA) samples as a teaching platform, an experimental teaching model driven by research tasks and clinical practice was established. The teaching design encompassed the entire workflow, including sample preparation, instrument operation, data processing, and result evaluation, enabling students to acquire hands-on experience with core LC-MS/MS techniques and quality control procedures. Through the implementation of the experimental project, students participated in EQA sample preparation, reference method-based quantification, homogeneity and stability assessments, and EQA result analysis, thereby gaining comprehensive exposure to the process from experimental design to result interpretation. The results demonstrated that the prepared EQA samples exhibited satisfactory homogeneity and stability, meeting the quality standards established by the China National Accreditation Service for Conformity Assessment (CNAS). In the \"2024 Beijing Serum Vitamin D EQA\" activity, a total of 16 medical laboratory institutions in Beijing participated. Teaching practice revealed that this project significantly enhanced students' comprehensive abilities in experimental design, instrument operation, data analysis, and quality assessment, while also fostering scientific thinking and teamwork. By introducing advanced analytical techniques into the undergraduate curriculum under the educational concept of \"research-driven teaching and integration of industry and education\", this approach not only optimized course content and experimental procedures but also broadened students' practical perspectives in clinical laboratory and research applications. This study provides a replicable teaching model for undergraduate laboratory education and offers valuable insights for promoting the integration of advanced analytical technologies into medical laboratory science training.</p>","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 3","pages":"363-370"},"PeriodicalIF":0.0,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12980505/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147438586","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}
{"title":"[Development of a liquid chromatography-tandem mass spectrometry method for steroid hormone detection during pregnancy and consistency analysis with chemiluminescence immunoassay].","authors":"Wei-Xiang Wu, Li-Hong Wu, Fu-Qiang Diao, You-Wen Luo, Chun-Ming Gu, Ming-Yong Luo","doi":"10.3724/SP.J.1123.2025.07001","DOIUrl":"10.3724/SP.J.1123.2025.07001","url":null,"abstract":"<p><p>Steroid hormones play a critical role in maintaining pregnancy and supporting fetal development. Accurate quantification of these hormones is essential for evaluating the endocrine status during pregnancy. While chemiluminescence immunoassay (CLIA) is widely used in clinical practice in China, it has inherent methodological limitations. In contrast, liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been internationally recognized for its superior analytical performance but remains underutilized in Chinese obstetric practice. Moreover, systematic evaluations comparing these two methods in pregnant women are still lacking. This study aimed to develop and validate an isotope-dilution LC-MS/MS method for the simultaneous quantification of four key steroid hormones, including cortisol, dehydroepiandrosterone sulfate (DHEAS), testosterone, and 17-hydroxyprogesterone (17-OHP). In addition, a consistency analysis was conducted between LC-MS/MS and CLIA among pregnant women. Method validation followed international bioanalytical guidelines, evaluating linearity, limits of quantification (LOQs), recovery, and precision. Serum samples from 94 pregnant women were collected at Guangdong Women and Children Hospital between January 2022 and December 2023, and were analyzed using both LC-MS/MS and CLIA. Method comparison was performed using paired <i>t</i>-tests, Pearson correlation, Bland-Altman plots, and Passing-Bablok regression to assess concentration differences, correlation, and systematic biases between the two methods. In this study, the established LC-MS/MS method exhibited excellent performance, with linear coefficients of determination >0.999, LOQs of 0.008-0.137 ng/mL, spiked recoveries of 92.1%-110.9%, and intra-assay relative standard deviations (RSDs) of 3.2%-9.0%, meeting the requirements for clinical detection. In a cohort of 94 pregnant women, paired <i>t</i>-tests revealed significant differences in hormone concentrations measured by LC-MS/MS and CLIA (all <i>P<</i>0.001). Specifically, LC-MS/MS yielded significantly lower values for cortisol (64.31 vs. 120.60 ng/mL) and DHEAS (532.44 vs. 1 612.1 ng/mL), but higher values for testosterone (1.10 vs. 0.88 ng/mL) and 17-OHP (2.00 vs. 1.07 ng/mL). Bland-Altman analysis further revealed obvious negative proportional biases for cortisol and DHEAS, with bias values of -56.29 ng/mL and -1 079.68 ng/mL, respectively. Additionally, the biases increased with the increase of concentration. In contrast, testosterone and 17-OHP showed positive biases, with bias values of 0.22 ng/mL and 0.89 ng/mL, respectively. The two methods showed extremely strong positive correlations in the detection of the four hormones (<i>P</i><0.001, <i>r</i>=0.819-0.974), among which the correlation of testosterone detection results was the highest (<i>r</i>=0.974). In the Passing-Bablok regression analysis, the consistency regression equation for cortisol was <i>C</i><sub>LC-MS/MS</sub>=-3.58+0.57<i>C</i><sub>C","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 3","pages":"257-266"},"PeriodicalIF":0.0,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12980516/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147439035","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}
{"title":"[Design of ZIF-L-based boronate affinity molecularly imprinted material and its application in the detection of ribavirin in environmental water].","authors":"Wanting Qi, Yukui Tong","doi":"10.3724/SP.J.1123.2025.04033","DOIUrl":"10.3724/SP.J.1123.2025.04033","url":null,"abstract":"<p><p>Ribavirin (RBV) is a broad-spectrum antiviral drug. It is widely used to treat various viral infections. However, its entry into water bodies can cause serious harm to both the ecological environment and human health. Thus, there is an urgent need for a simple and efficient method to detect RBV for detection purposes. In this study, a two-dimensional ZIF material (ZIF-L) served as the matrix, RBV as the template molecule, and 3-aminophenylboronic acid (APBA) as the functional monomer, using its self-polymerization ability to form a molecularly imprinted layer on the surface of ZIF-L. Imprinted cavities were created using a MeOH-HAc (1∶1, volume ratio) eluent to disrupt the interaction between RBV and APBA, yielding ZIF-L-based boronate affinity molecularly imprinted polymers (ZIF@B-MIPs). Non-imprinted materials (ZIF@B-NIPs) were prepared identically without RBV. ZIF@B-MIPs features dynamic recognition sites formed through pH-responsive boronate ester bonds. This enabled synergistic recognition based on the template molecule's \"shape memory\" and \"chemical bonding\". Scanning electron microscopy (SEM) and Fourier-transform infrared spectroscopy (FT-IR) were employed to characterize the morphology and functional groups of the material. Notably, new FT-IR peaks emerged for ZIF@B-MIPs at 1 381 cm<sup>-1</sup> (B-O vibration) versus ZIF-L, confirming APBA polymerization. This indicates that the polymerization of APBA onto the surface of ZIF-L was successful. The synthesis and adsorption conditions were optimized. The results showed that, with a ZIF-L dosage of 100 mg, the optimal amount of the self-polymerizing reagent APBA was 100 mg. A self-polymerization time of 5 h was sufficient to form an appropriately thick imprinted layer. At pH 8.5, the stability of the polymer network was maintained while the imprinting effect and mass transfer efficiency were maximized. The post-elution re-adsorption capacity retention rate reached 96.8%, balancing elution efficiency with structural integrity. A RBV mass concentration of 60 mg/L was selected for the experimental requirements. After optimization, the saturation adsorption capacity of ZIF@B-MIPs for RBV reached 21.43 mg/g. The imprinting factor (IF) was 5.32. The material's performance was assessed through adsorption and reusability experiments. The results indicated that the material possesses good specificity and selective recognition ability. It also exhibits a rapid adsorption rate and good reusability. The adsorption experiment results showed that the adsorption kinetics followed the pseudo-second-order model (<i>R</i><sup>2</sup>=0.995 3). Adsorption equilibrium was achieved within 15 min. The adsorption process of RBV by the adsorbent involves chemisorption. The Langmuir isotherm adsorption model (<i>R</i><sup>2</sup>=0.982 5) fitted the experimental data better. This indicates that the adsorption of RBV by ZIF@B-MIPs likely involves monolayer adsorption. In mixed solutions of RBV and three interf","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 2","pages":"214-222"},"PeriodicalIF":0.0,"publicationDate":"2026-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12878565/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146121744","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}