JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2024
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IF 2.8
Xijin Yang,Ying Li,Qiju Shao,Zhirong Li,Zeli Chun,Yan Wang,Yaping Zhou,Rongxiang Chen
Persicaria chinensis (L.) H. Gross ( P. chinensis ), also known as “Huotanmu” in Chinese, is a traditional ethnic herbal medicine and a functional food ingredient. In this study, liquid chromatography − electrochemical detection (LC-ECD) screening, liquid chromatography − tandem mass spectrometry (LC-MS/MS) identification, and multivariate statistical analysis were combined to clarify the antioxidant components in P. chinensis . The samples were extracted using 80 % aqueous methanol under ultrasound-assisted extraction and their in vitro antioxidant activities were evaluated. The fingerprint of P. chinensis was established using LC-ECD, while the identification of major chemical components was performed using LC-MS/MS through comparison of ion fragments. Subsequently, grey correlation analysis and partial least squares regression analysis were used to investigate the association of different compounds with antioxidant activity. P. chinensis from different sources showed excellent DPPH radical scavenging capacity, ABTS radical scavenging capacity, and ferric reducing antioxidant power. A total of 25 common peaks were obtained and identified in the LC-ECD fingerprint of P. chinensis , which were primarily comprised of tannins and flavonoids. The similarity between samples of different batches was ≥ 0.767, indicating relatively consistent quality. The comprehensive analysis results of grey relational analysis and partial least squares regression analysis indicated that tannins such as di-galloyl-HHDP-hexoside and davidiin were the major contributors to the antioxidant activity of P. chinensis . Therefore, LC-ECD can rapidly screen the potential phenolic antioxidants of P. chinensis , providing a basis for its product development, resource utilization, and quality control.
研究领域:
植物化学
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药理学
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分析化学
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PubMed
高影响因子
ANALYTICA CHIMICA ACTA
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2026
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IF 6
Xingyu Shi,Xuan Liang,Shuilin Xie,Ting Zhou,Wei Xiong
Background Fatty acids (FAs) are essential metabolites involved in energy storage, signaling, and inflammation regulation, and their biological functions are closely linked to the position and geometric configuration of carbon–carbon double bonds (C C). However, the isomer-resolved characterization and highly sensitive detection of FAs in complex biological matrices remain challenging due to their co-elution, similar fragmentation, and low ionization efficiency. Therefore, there remains a critical need for an efficient approach that can simultaneously enhance chromatographic separation, enable unambiguous C C characterization, and improve detection sensitivity for FA isomers in biological samples. Results In this study, we developed a double derivatization strategy combining magnesium monoperoxyphthalate hexahydrate (MMPP) epoxidation with N,N-diethyl-1,2-ethanediamine (DEEA) amidation, coupled with LC–MS/MS, for isomer-resolved FA analysis. The double derivatization enhanced the chromatographic resolution of positional and cis/trans isomers, enabled reliable localization of C C positions via Δ16 Da diagnostic ion pairs, and improved detection sensitivity by 16–32 fold relative to epoxidation alone. Cis -trans configurations were further supported by parallel linear relationships between retention time and C C position under identical LC conditions, providing a standards-sparing criterion for structural assignment. Applied to mouse plasma, the strategy identified 69 FAs, including 55 unsaturated species, representing an increase of 46 over the underivatized approach. Quantitative analyses and differential analyses showed most FAs were elevated in hepatitis B virus (HBV) mice, with altered isomer ratios pointing to disrupted desaturase activity and oxidative stress. Significance In conclusion, this double derivatization LC-MS/MS platform provided improved structural resolution, higher detection sensitivity, and more reliable configurational assignment of FAs without requiring extensive standards. Its successful application to HBV mouse plasma demonstrated its suitability for complex biological matrices and highlighted its potential for biomarker discovery and mechanistic studies of lipid-related metabolic diseases.
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高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2026
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IF 3.4
Kun Yang,Jianhua Wu,Chengming Yang,Liang Liu
A Protein G magnetic bead-based LC-MS/MS method was developed for dupilumab quantification in human serum. • The surrogate peptide SGQSPQLLIYLGSNR enabled sensitive and specific targeted detection (LLOQ 1.00 µg/mL). • Excellent linearity, precision and accuracy were achieved across a wide dynamic range (1.00–400 µg/mL). • Considerable interpatient variability was observed in clinical trough samples. Dupilumab, a monoclonal antibody targeting IL-4Rα, is used for the treatment of type 2 inflammatory diseases. Recent studies have revealed a nonlinear relationship between its serum concentration and clinical response, particularly a “biological tipping point” during dose interval prolongation, highlighting the need for individualized therapeutic drug monitoring (TDM). In this study, a robust liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for dupilumab quantification in human serum was developed and validated. Specifically, dupilumab was enriched from 50 µL serum using Protein G magnetic beads, followed by denaturation, reduction, alkylation, and tryptic digestion. A surrogate peptide SGQSPQLLIYLGSNR was selected for quantification, and its stable isotope-labeled (SIL) analog served as an internal standard. Separation was performed on an Acquity UPLC BEH C 8 column (50 mm × 2.1 mm, 1.7 µm) with detection using positive electrospray ionization in multiple reaction monitoring (MRM) mode. Excellent linearity was achieved from 1.00 to 400 µg/mL (r² > 0.99), with a lower limit of quantification of 1.00 µg/mL. Intra- and inter-run precision (%CV) and accuracy (%Bias) were within 9.27%. The validated method was successfully applied to analyze clinical serum samples. The established LC-MS/MS method provides a reliable alternative to immunoassays, with a wide dynamic range suitable for TDM and personalized dose interval adjustments in patients receiving dupilumab. Download: Download high-res image (93KB) Download: Download full-size image
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高影响因子
Frontiers in Chemistry
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2024
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IF 3.8
Baodong Feng,Linqi Su,Yang Yang,Renyan Liu,Yu Zhang,Lingyi Xin,Li Wang,Zhiming Yang,Xuemei Wei,Qinhua Chen
Background: Ulcerative colitis (UC) is a chronic inflammatory bowel disease (IBD) influenced by multiple factors. Berberine, an isoquinoline alkaloid derived from the root and bark of Coptis chinensis Franch., has shown promise in managing UC, but its underlying mechanisms remain unclear.Methods: To elucidate the relationship between berberine, ulcerative colitis (UC), and the organism’s metabolome, we established a dextran sulfate sodium (DSS)-induced UC model in rats. Colonic tissue was collected for histopathological examination, while plasma samples were analyzed using liquid chromatography-tandem mass spectrometry (LC-MS/MS) with dynamic Multiple Reaction Monitoring (dMRM). This approach, characterized by its short analysis time of 20 min per sample, excellent reproducibility, and straightforward data processing, allowed for the comprehensive detection of a wide array of metabolites, including amino acids, lipids, and organic acids, many of which are implicated in the pathophysiology of UC.Results: Our results showed that berberine modulated the metabolic disturbances of 33 compounds in the plasma of UC rats, primarily including amino acids, pyrimidines, organic phosphoric acids, fatty acyls, and organonitrogen compounds. These altered metabolites were associated with various pathways, such as amino acid metabolism, glutathione metabolism, nicotinate and nicotinamide metabolism, taurine and hypotaurine metabolism, pyrimidine metabolism, glyoxylate and dicarboxylate metabolism, and the citrate cycle (TCA cycle). Notably, 3-hydroxyproline, homocysteic acid, L-threonine, L-lysine, carbamoyl phosphate, O-phosphoethanolamine, taurine, leucine, and phosphorylcholine exhibited significant differences between the Treatment and Model groups, with levels reverting to those of the Control group (p < 0.001). These findings suggested that these compounds may serve as potential plasma biomarkers for UC.Conclusion: This study provided valuable insights into the mechanism by which berberine exerted its therapeutic effects on UC through metabolomics. Our results highlighted berberine’s potential to modulate key metabolic pathways and restore the levels of several metabolites, suggesting its utility as a therapeutic agent for UC. These findings underscored the importance of metabolomics in understanding the pathophysiology and treatment of UC.
研究领域:
药理学
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代谢组学
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炎症性肠病研究
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PubMed
高影响因子
XENOBIOTICA
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2025
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IF 1.2
Shanshan Chen,Donghan Wang,Yuanyuan Zhao,Yaqi Sun,Yueyao Luan,Qixuan Sun,Jiaqi Wang,Yuhang Yan,Jing Yu,Chunhua Zhou
With the increasing prevalence and escalating complexity of mental disorders, precise medication has become critically important. This necessitates an efficient, accurate, and convenient method for drug concentration monitoring to support laboratory personnel and clinicians. In this study, three liquid chromatography-tandem mass spectrometry methods were developed and validated for simultaneously determining and quantifying 27 antipsychotics and related metabolites in human plasma. The plasma samples were subjected to protein precipitation using methanol, with isotope-labelled internal standards (ISs), followed by separation via isocratic elution on a BEH C18 column. Mass spectrometric analysis was performed using electrospray ionisation in positive ionisation mode with multiple reaction monitoring for quantitative detection. The analytes demonstrated high separation efficiency, with a single sample run time of 3.0 min. The method exhibited a wide linear range with excellent linearity across the concentration range. The intra- and inter-batch precision were ≤10.00%, the accuracy was 88.67–113.29%. Accurate quantification of antipsychotics remained unaffected under various storage conditions: 72 h at room temperature, 7 d at 4 °C refrigeration, and 14 d at −80 °C freezing. This validated methodology has been successfully applied to plasma samples from patients with psychiatric disorders, demonstrating its practical utility for accurate quantification of antipsychotics in large-scale and complex matrices containing multiple analytes.
研究领域:
临床医学
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分析化学
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PubMed
高影响因子
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
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2024
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IF 4
Can Cui,Xiaojun Jiao,Xianbin Xu,Jiongzhou Gong,Jiaxin Zhou,Ge Tian,Liwei Lu,Li Li,Xianhui Huang
The presence of residues of veterinary drugs in eggs is an ongoing and significant issue of concern. Fluralaner is widely used in the prevention of ectoparasites, including the poultry red mite, but no analytical method has been reported for detection of its residues in eggs. An HPLC-MS/MS method was established for the determination of fluralaner residues in whole eggs and validated for LOD, LOQ, specificity, linearity, accuracy, precision, and matrix effects. LOD was 5 μg•kg −1 and LOQ was 65 μg•kg −1 . Recovery ranged from 97.7% to 103.7% (spiked at 65, 650, 1300, and 2600 μg•kg −1 ), while intra-assay and inter-assay coefficients of variation were consistently below 1.5%. A drug withdrawal trial was conducted with 16 laying hens administered a therapeutic dose of fluralaner in drinking water on days 0 and 7, with eggs being analyzed for 23 days. The highest concentration, 1235 μg•kg −1 , was detected on day 13. This was below the European Union maximum residue limit for fluralaner in edible chicken tissues and eggs (1300 μg•kg −1 ). Residues were detectable up to two weeks after cessation of treatment. This method is suitable for routine compliance monitoring of fluralaner residues in egg matrices and may be adapted for analysis of other edible tissues.
研究领域:
兽医学
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食品科学
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高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2024
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IF 3.1
Mengru Bai,Qian Shen,Yong Wu,Zhiyuan Ma,Yuqing Wang,Mingyang Chen,Dan Liu,Lin Zhou
Methotrexate (MTX) is commonly prescribed as the initial treatment for gestational trophoblastic neoplasia (GTN), but MTX monotherapy may not be effective for high-risk GTN and choriocarcinoma. The cellular uptake of MTX is essential for its pharmacological activity. Thus, our study aimed to investigate the cellular pharmacokinetics and transport mechanisms of MTX in choriocarcinoma cells. For the quantification of MTX concentrations in cellular matrix, a liquid chromatography-tandem mass spectrometry method was created and confirmed initially. MTX accumulation in BeWo, JEG-3, and JAR cells was minimal. Additionally, the mRNA levels of folate receptor α (FRα) and breast cancer resistance protein (BCRP) were relatively high in the three choriocarcinoma cell lines, whereas proton-coupled folate transporter (PCFT), reduced folate carrier (RFC), and organic anion transporter (OAT) 4 were low. Furthermore, the expression of other transporters was either very low or undetectable. Notably, the application of inhibitors and small interfering RNAs (siRNAs) targeting FRα, RFC, and PCFT led to a notable decrease in the accumulation of MTX in BeWo cells. Conversely, the co-administration of multidrug resistance protein 1 (MDR1) and BCRP inhibitors increased MTX accumulation. In addition, inhibitors of OATs and organic-anion transporting polypeptides (OATPs) reduced MTX accumulation, while peptide transporter inhibitors had no effect. Results from siRNA knockdown experiments and transporter overexpression cell models indicated that MTX was not a substrate of nucleoside transporters. In conclusion, the results indicate that FRα and multiple transporters such as PCFT, RFC, OAT4, and OATPs are likely involved in the uptake of MTX, whereas MDR1 and BCRP are implicated in the efflux of MTX from choriocarcinoma cells. These results have implications for predicting transporter-mediated drug interactions and offer potential directions for further research on enhancing MTX sensitivity.
研究领域:
药理学
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肿瘤学
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细胞生物学
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分析化学
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PubMed
高影响因子
RSC Advances
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2017
·Vol. 7
·期 67
·42073-42082
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IF 3.108
Ling-Yuan Guo,Shu-Zhen Yan,Qiang Li,Qiao Xu,Xi Lin,Shan-Shan Qi,Shu-Qin Yu,Shuang-Lin Chen
Hypocrellin A (HA), a perihydroxylated polycyclic quinone isolated from the fungus of Shiraia bambusicola, exhibits a wide spectrum of biological activities in pre-clinical studies. However, poor water solubility is a major clinical constraint factor of HA, leading to unpredictable bioavailability. In this study, HA-loaded poly (lactic-co-glycolic acid) (PLGA) nanoparticles (PLGA/HA NPs) were prepared by the single-emulsion solvent-evaporation technique. Characterization of PLGA/HA NPs showed that HA was successfully encapsulated on the PLGA. The drug-loading content and encapsulation efficiency (EE) were 7.0% and 57.5%, respectively. The in vitro release profile demonstrated that HA was released more slowly from nanoparticles in pH 1.5 and pH 6.8 than in pH 7.4. Furthermore, the highest solubility of PLGA/HA NPs in aqueous solution was approximately 35.67-fold that of native HA (n-HA). PLGA/HA NPs had more superior stability compared with n-HA in physiological conditions. In this paper, a sample and sensitive LC-MS/MS method was validated for the first time to quantify HA in rat plasma. The pharmacokinetic parameters and bioavailability of HA between PLGA/HA NPs and n-HA were compared after oral administration in rat. The results implied that the relative bioavailability of PLGA/HA NPs was 2.67-fold that of n-HA, and PLGA/HA NPs had a longer half-life. Therefore, these results suggested that PLGA-blend nanoparticles improved the solubility, stability and bioavailability of HA, and could become a potential and promising carrier for the oral delivery of HA.
研究领域:
药学
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纳米技术
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药物递送系统
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高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2025
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IF 3.1
Chenchen Jiang,Siqi Chen,Min Huang,Xiaojiao Yi,Haiying Ding,Junfeng Zhu,Luo Fang
Doxorubicin (DOX) is an effective chemotherapeutic agent, but its use is limited by dose-dependent cardiotoxicity. Palmatine (PAL) has shown potential in preventing doxorubicin-induced cardiotoxicity (DIC); however, the underlying mechanism remains unclear. Since DOX accumulation in cardiomyocytes is a key factor in the development of cardiotoxicity, this study aims to explore the pharmacokinetic mechanisms through which PAL alleviates DIC. First, the effect of PAL on DIC was assessed based on H9c2 cardiomyocytes model using sulforhodamine B (SRB), lactate dehydrogenase (LDH), flow cytometry and Western blot assays, which demonstrated that PAL significantly attenuated DOX-induced cardiac toxicity and apoptosis. Second, a sensitive and efficient LC–MS/MS method was established to quantify DOX in H9c2 cells, with a lower limit of quantification of 10 nM and a total run time of 4 min per sample. Cellular pharmacokinetic study revealed that PAL significantly reduced DOX concentration in H9c2 cells. Finally, molecular docking analysis revealed that PAL exhibited low binding energies and formed hydrogen with uptake transporter proteins involved in DOX transport in cardiomyocytes, including organic cardi transporter (OCT) 1, OCT3, organic cation/carnitine transporter (OCTN) 1, OCTN2, and plasma membrane monoamine transporter (PMAT). This suggests a stable interaction between PAL and these transporters. In conclusion, PAL alleviates DIC, most likely by reducing myocardial DOX accumulation through the inhibition of uptake transporters. This study provides novel pharmacokinetic insights into the mechanism by which PAL mitigates DIC and underscores its potential as a complementary therapeutic agent in combination with DOX in clinical applications.
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高影响因子
CLINICA CHIMICA ACTA
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2025
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IF 2.9
Ying Shen,Xia Luo,Qing Guan,Liming Cheng
Background The quantification of urinary oxalate is essential for the diagnosis of primary hyperoxaluria. This study sought to develop a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for urinary oxalate determination and to evaluate its concordance with an established in-house high-performance liquid chromatography (HPLC) method and a commercial LC-MS/MS assay. Methods The newly developed LC-MS/MS method invloved the quantification of urinary oxalate through a straightforward single-step derivatization process using o -phenylenediamine at 120 °C for 20 min. A total of 291 urine samples were analyzed using both the in-house LC-MS/MS and HPLC methods, while 94 urine samples were evaluated using both our in-house LC-MS/MS method and a commercial LC-MS/MS assay. Additionally, a reference interval for 24-hour urinary oxalate in Chinese adults was established. Results Oxalate exhibited strong analytical retention in reverse-phase liquid chromatography. The newly developed LC-MS/MS method demonstrated excellent linearity with a correlation coefficient exceeding 0.995, and acheived recovery rates ranging from 92.80 % to 98.73 %. The intra-assay and inter-assay coefficients of variation (CVs) were between 0.79 % to 7.46 %, with a total CV ranging from 2.07 % to 7.50 %. No significant matrix effect was observed. However, discrepancies were identified between the in-house LC-MS/MS method and both the commercial LC-MS/MS assay and the HPLC method. The reference interval was established at 0.12–1.04 mmol/24 h (10.8–93.6 mg/24 h). Conclusions The developed LC-MS/MS method is robust and simple, providing a reliable tool for the clinical assessment of urinary oxalate. An accurate method is essential for screening analyses in primary hyperoxaluria.
研究领域:
临床化学
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分析化学
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代谢性疾病
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实验医学
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质谱分析
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PubMed
高影响因子
CHEMICO-BIOLOGICAL INTERACTIONS
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2026
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IF 5.2
Huan-le Ye,Xin-xin Zheng,Mian-mian Li,Zhi-qiang Zhang,Liu-xu Chen,Wen-jing Zhang,Ren Cheng-Han Fan,Guo-xin He,An-cong Xu
Aims This study aimed to elucidate the biochemical and metabolic mechanisms underlying glufosinate-ammonium-induced neurotoxicity, with a focus on brain metabolic disturbances. Methods Male Sprague-Dawley rats were administered glufosinate-ammonium by intragastric gavage, with saline-treated animals serving as controls. Neuropathological changes and cognitive performance were assessed at 2 and 6 days post-exposure. Oxidative stress and energy metabolism were evaluated by measuring plasma antioxidant indices, and brain levels of superoxide dismutase (SOD), glutathione (GSH/GSSG), total antioxidant capacity (T-AOC), and adenosine triphosphate (ATP). In addition, untargeted LC-MS/MS-based metabolomics of brain tissue was conducted to characterize exposure-related metabolic perturbations. Results Histopathological examination revealed marked brain injury on day 2 post-exposure, characterized by neuronal necrosis, apoptosis, and severe mitochondrial disruption. Although pathological severity was attenuated by day 6, residual cellular damage remained evident. Behavioral testing revealed significant impairments in spatial learning and memory in the glufosinate-ammonium-exposed group. Biochemical analyses revealed disrupted oxidative stress and energy metabolism, reflected by altered levels of superoxide dismutase (SOD), glutathione (GSH/GSSG), total antioxidant capacity (T-AOC), and adenosine triphosphate (ATP) in brain tissue. Metabolomic analysis revealed pronounced alterations in brain metabolic profiles, involving pathways related to oxidative stress, energy metabolism, and amino acid metabolism. Early-stage disturbances were dominated by alterations in glutamate and tricarboxylic acid (TCA) cycle-related metabolites, whereas later-stage changes primarily involved taurine and hypotaurine metabolism. Conclusion Following glufosinate-ammonium exposure, rats exhibited neurological dysfunction and cognitive impairment, accompanied by metabolic disturbances in brain tissue, particularly in oxidative stress, energy metabolism, and amino acid metabolism. These findings provide mechanistic insight into glufosinate-ammonium-induced neurotoxicity and highlight the critical role of metabolic dysregulation.
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高影响因子
ANALYTICAL CHEMISTRY
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2019
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IF 6.35
Ning Zhang,Wenchao Deng,Yao Li,Yangde Ma,Yan Liu,Xiangjun Li,Hailin Wang
Cyclobutane pyrimidine dimers (CPDs) and pyrimidine (6–4) pyrimidone photoproducts (6–4PPs) are genotoxic DNA lesions and mainly generated on thymine–thymine (T–T) dinucleotides upon UV irradiation. Regarding the sensitivity, specificity, and accuracy of analytical methods, it is of first choice to develop a reliable assay for simultaneous detection of these DNA lesions using liquid chromatography-tandem mass spectrometry (LC-MS/MS). However, the dilemma is the low detection sensitivity of the phosphate-containing dimeric photoproducts even using most favorable negative-ion mode for LC-MS/MS analysis. Unexpectedly, we observed that the detection sensitivity of T–T CPD and 6–4PP could be significantly improved using formic acid/acetic acid (∼ppm) as an additive of the mobile phase for reversed-phase LC-MS/MS analysis. This is the first demonstration of the enhancement of LC-MS/MS signals by formic acid/acetic acid in negative-ion mode. Of note, these acidic agents are often used for positive-ion mode in LC-MS assays. Benefited from the developed method, we could quantify both T–T CPD and 6–4PP in mouse embryonic stem cells upon UVC irradiation at low dosage. This sensitive method is applicable to the screening and identification of genes involved in formation, signaling, and repair of UV lesion.
研究领域:
生物化学
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分子生物学
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分析化学
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PubMed
高影响因子
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