BMC Chemistry
·
2026
·
IF 5.1
Yang Xiaoyu,Zhao Chaoyue,Ding Yiwen,Li Yining,Zhao Yushang,Lin Wanling,Li Jing,Wang Dong,Yue Zhihong,Pei Lin,Jia Mei,Cao Lin-Lin,Wang Hui
With the global spread of antimicrobial resistance (AMR), infections caused by multidrug-resistant bacteria have become a major challenge in clinical treatment. ‘Imipenem, Cilastatin Sodium and Relebactam for Injection’ is a critical therapeutic agent for treating infections caused by multidrug-resistant Gram-negative bacteria. However, it is associated with gastrointestinal adverse reactions, necessitating therapeutic drug monitoring (TDM) for precise dosing. Currently, there is no method for simultaneously detecting the concentrations of all three components in ‘Imipenem, Cilastatin Sodium and Relebactam for Injection’. Therefore, this study established an analytical method based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the simultaneous quantification of imipenem, relebactam, and cilastatin in serum, urine, and peritoneal drainage fluid (PD). After protein precipitation, samples were separated using a CORTECS ® HILIC column with 5 mM ammonium acetate aqueous solution-acetonitrile as the mobile phase for gradient elution, detected in positive electrospray ionization (ESI+) mode. This LC-MS/MS method showed excellent linearity (R² > 0.99) for all three drugs, and the linearity ranges had well met the clinical requirements. The limits of quantification (LOQ) were 40 ng/mL (serum/ PD) and 80 ng/mL (urine), and the carryover contamination rate was < 0.1%. All intra-day and inter-day coefficients of variation (CVs) were < 15%, the recovery rates ranged from 89.7% to 103.2%, and the matrix effects were acceptable (87.7%–110.8%). In conclusion, this LC-MS/MS method is simple to operate, exhibits high sensitivity and accuracy, and meets the requirements for the TDM of ‘Imipenem, Cilastatin Sodium and Relebactam for Injection’, providing support for individualized treatment and reducing the risk of adverse reactions.
✓ 已验证
DOI
PubMed
高影响因子
Analytical Methods
·
2026
·
IF 3
Chujun Liu,Jiankang Ren,Qian Ran,Yuliang Xu,Boyan Sun,Zhiyue Feng,Sihan Wang,Jie Xie,Haiyang Jiang
Conventional multiple reaction monitoring (MRM) quantification of β-agonists in complex matrices was hindered by insufficient sensitivity due to co-extracted matrix interferences. To address this drawback, we developed a highly selective and specific liquid chromatography triple-stage tandem mass spectrometry (LC-MS/MS/MS, LC-MS3) method via systematic comparison of MRM and MRM3 modes for the determination of nine β-agonists (ractopamine, penbutolol, cimaterol, salbutamol, clenbuterol, tulobuterol, clorprenaline, terbutaline, fenoterol) in high-fat milk and pork. MS3 method overcomes the limitations of conventional MS/MS through the multi-stage fragmentation capability of a hybrid linear ion trap (LIT), enabling deeper structural characterization and superior matrix interference resistance. The results demonstrated that LC-MS3 method not only accurately quantified β-agonists in complex matrices, but also significantly enhanced sensitivity by reducing matrix effects. Extracted ion chromatograms (XICs) revealed nearly interference-free peaks, exhibiting the excellent selectivity and specificity of the LC-MS3 method. The LC-MS3 method exhibited good linearity (R² ≥ 0.9973), and the limits of detection (LOD) and quantification (LOQ) for β-agonists ranged from 0.01 to 0.05 μg/kg and 0.03 to 0.15 μg/kg, respectively. The recoveries were between 85.47% and 105.32%, with intra-day and inter-day relative standard deviations (RSDs) of 1.68%–6.42% and 2.42%–8.68%, respectively. The matrix effect (ME) was within -10.55% to 9.53%. In comparison, the conventional LC-MS/MS method showed higher LODs (0.1–0.15 μg/kg), LOQs (0.3–0.45 μg/kg), and broader matrix effects (-18.12%–19.35%), confirming the superior sensitivity of the LC-MS3 method. This is the first study to employ MRM3 mode for the determination of β-agonists in high-fat milk and pork matrices.
✓ 已验证
DOI
PubMed
高影响因子
Talanta Open
·
2026
·
IF 5.1
Jie Fu,Yong Shao,Hua Shao,Guo Jingyuan,Tangwei Zhang,Jin Fen,Jing Wang,A.M. Abd El-Aty,Yongxin She
A rapid, sensitive, and reliable method was developed for the determination of six dinocap phenol isomers in 23 plant-derived foods via a modified QuEChERS approach coupled with liquid chromatography‒tandem mass spectrometry (LC‒MS‒MS/MS). Chromatographic and mass spectrometric conditions were optimized, and the separation performance of eight chromatographic columns was systematically evaluated to achieve effective isolation of the six dinocap phenol isomers. The method was validated on the basis of maximum residue limits (MRLs) across 23 matrices, with spiked levels ranging from 0.003 to 0.3 mg/kg. The average recoveries were between 60% and 112%, with relative standard deviations (RSD) less than 21%. The limits of quantification (LOQs) ranged from 0.003 to 0.015 mg/kg. This method successfully addressed challenges in the detection of dinocap phenols by enabling clear and precise separation of individual isomers while mitigating matrix effects through matrix-matched calibration.This study contributes to global efforts to increase food safety, support sustainable agricultural practices, and promote public health through improved methods for detecting and managing pesticide residues.
✓ 已验证
DOI
高影响因子
Metabolites
·
2026
·Vol. 16
·期 8
·543
·
IF 4.5
Yan Yan,Jiaying Liu,Yingjian Deng,Yu Tao,Xinxin Li,Chenhui Du,Kun Yang,Ruiping Zhang
Objectives:Insomnia is a highly prevalent sleep disorder involving complex neurochem-ical dysregulation; however, the spatial distribution of neurotransmitters and small-molecule metabolites across distinct brain microregions in the insomniac state re-mains poorly characterized. This study aimed to map region-specific metabolic perturba-tions in situ in a p-chlorophenylalanine (PCPA)-induced insomnia rat model using opti-mized matrix-assisted laser desorption/ionization mass spectrometry imaging (MAL-DI-MSI) integrated with targeted metabolomics validation.Methods:On-tissue chemical derivatization MALDI-MSI was optimized using α-cyano-4-hydroxycinnamic acid (CHCA) as the matrix on a Bruker tims TOF flex mass spectrometer. The rats received PCPA (400 mg/kg, intraperitoneal) for three days to establish the insomnia model. Metabolite identifi-cation was conducted using MetaboScape® software (2020b) and the Human Metabolome Database. Ultra-performance liquid chromatography–tandem mass spectrometry was em-ployed to quantify nine key neurotransmitters and metabolites across six brain microre-gions. Key synthetic enzyme expression was evaluated by immunofluorescence and West-ern blotting analyses.Results:TMP-TFB-derived brain slices clearly showed the distribu-tion of neurotransmitters in brain microregions. MALDI-MSI demonstrated that the spatial distribution and abundance of eight neurotransmitters were disturbed in brains of PCPA-induced insomniac rats. A total of 346 metabolites were characterized across six brain microregions (cerebellum, cortex, hippocampus, brainstem, hypothalamus, and stri-atum), with principal coordinate analysis revealing clear metabolic separation between control and insomniac rats. PCPA treatment markedly disrupted tryptophan and tyrosine metabolism, evidenced by decreased 5-HT, 5-HTP, and 5-HIAA, alongside region-specific alterations in DA, NE, HVA, and Ach. Additionally, GABA levels decreased in the hippo-campus, striatum, and hypothalamus, whereas glutamate increased throughout the brain. Targeted metabolomics validated the MSI findings, and Bland–Altman analysis confirmed good consistency between the two analytical platforms. PCPA further disturbed the meta-bolic enzymes MAOA, DDC, and TPH2 within the Trp-5-HTP-5-HT-5-HIAA metabolic pathway in the brainstem and TYH and DBA within the tyrosine-DA-NE metabolic pathway in the striatum.Conclusions:This study demonstrates that region-specific altera-tions in tryptophan and tyrosine metabolism pathways provide mechanistic insights into insomnia pathogenesis and potential therapeutic targets.
✓ 已验证
产品关联
DOI
高影响因子
Frontiers in Nutrition
·
2025
·
IF 5.1
Shuo Diao,Guanrong Feng,Yixuan Wang,Jingming Ma,Zhihua Lv,Mingming Yu,Yue Sun
Objective: In this study, a highly selective and sensitive LC-MS/MS method was developed to comprehensively analyze the distribution of astaxanthin across various tissues of Litopenaeus vannamei, as well as its variations in the hepatopancreas and ovary throughout ovarian development.Methods: The separation was performed on a BEH C8 column (1.7 μm, 2.1 × 50 mm) using a a gradient elution. The initial mobile phase composition was 0.1% formic acid in 3 mM ammonium acetate in water (solvent A) and methanol (solvent B) at a ratio of 15:85 (v/v), with a flow rate of 0.20 mL/min.Results: The assay demonstrated linearity over a concentration range of 20 to 10,000 ng/mL, with accuracy varying from −0.1 to 1.7% and precision within 2.1%. Using the established methodology, astaxanthin concentrations were quantitatively analyzed and comparatively assessed across various tissues of L. vannamei. Analytical results demonstrated that the ventral nerve cord and hepatopancreas exhibited the highest astaxanthin concentrations among all examined tissues, with values of 351 μg/g and 116 μg/g, respectively. During the ovarian developmental stages, astaxanthin was predominantly sequestered in the hepatopancreas during early phases, with concentrations ranging from 21.3 μg/g to 29.1 μg/g, representing a 43- to 59-fold increase compared to ovarian concentrations. However, a significant redistribution of astaxanthin was observed during the post-developmental stage, characterized by a substantial decrease to 5.74 μg/g in the hepatopancreas, concomitant with an increase to 7.47 μg/g in ovarian tissue.Conclusion: This validated LC-MS/MS method effectively quantified astaxanthin in various tissues of Litopenaeus vannamei, providing new insights into its tissue-specific distribution and potential role during ovarian development.
✓ 已验证
产品关联
DOI
PubMed
高影响因子
BMC Chemistry
·
2025
·Vol. 19
·期 1
·180
·
IF 4.6
Xiaoyu Yang,Wanling Lin,Yushang Zhao,Chaoyue Zhao,Fei Zhou,Dong Wang,Zhihong Yue,Lin Pei,Mei Jia,Bin Cao,Lin-Lin Cao,Hui Wang
“Xiannuoxin” (simnotrelvir/ritonavir) is a novel anti-severe acute respiratory syndrome coronavirus 2 (SARS-CoV-2) drug developed in China, which plays an antiviral role by inhibiting 3C-like protease (3CL pro ). At present, it has been put into clinical use, while a simple, accurate and sensitive detection method is urgently needed for the quantification of simnotrelvir/ritonavir in human serum and bronchoalveolar lavage fluid (BALF) to ensure safe and efficacious antiviral therapeutics. In this study, we developed a liquid chromatography tandem mass spectrophotometry (LC-MS/MS) method for the simultaneous determination of simnotrelvir, ritonavir and urea concentrations in human serum and BALF samples. Prior to LC-MS/MS analysis, a user-friendly, one-step pre-analytical process was conducted, followed by a rapid chromatographic run lasting 3 min. This was then succeeded by positive and negative electrospray ionization and detection using a triple quadrupole tandem mass spectrometer in the multiple reaction monitoring mode. Subsequently, the LC-MS/MS method underwent a comprehensive validation in aspects such as sensitivity (LoQs of 2.5 ng/mL, 0.1 ng/mL, and 1 μg/mL for simnotrelvir, ritonavir and urea), linearity, carryover, precision, trueness (recovery rates of simnotrelvir, ritonavir and urea were between 85 and 115%), matrix effect (within 85-115%) and stability (stable for 72 h at room temperature). The validation results demonstrated that this LC-MS/MS method was robust and reliable. Notably, we can use the urea dilution correction method to calculate the concentrations of simnotrelvir and ritonavir in epithelial lining fluid (ELF), which is of great significance for evaluating the effectiveness and safety of antiviral drug treatment.
研究领域:
药理学
·
分析化学
·
病毒学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Dong Wang,Mengrong Li,Tingting Dai,Xiangyu Zhang,Di Chen
A rapid, sensitive, and green sample preparation method based on polypropylene fiber-supported liquid-phase microextraction followed by liquid chromatography–tandem mass spectrometry was developed for the determination of tyrosine kinase inhibitors in plasma. Commercial oil absorbent pads composed of polypropylene fibers were used to support n-octanol as the extraction phase. The high chemical purity of the polypropylene fiber minimized background interference, enabling reliable trace-level analysis. The in-syringe format allowed simple push–pull operation, and extraction conditions were optimized for maximum efficiency. The method demonstrated excellent linearity (R 2 > 0.995), low limits of quantification (0.067–3.0 ng/mL), and high precision, with intra- and inter-day recoveries ranging from 79.5 % to 113.6 % and relative standard deviations below 14.2 %. A blinded spiked sample analysis confirmed the method’s reliability for clinical application. The greenness of the method, as evaluated by five green assessment tools, demonstrated excellent environmental compatibility. Overall, the proposed in-syringe polypropylene fiber-supported liquid-phase microextraction method offers a simple, cost-effective, and environmentally sustainable solution for the analysis of tyrosine kinase inhibitors in complex biological matrices.
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2023
·
IF 3
Zheyue Bo,Wanjun Han,Haoyue Zhao,Han Liu,Ting Liang,Lanjing Li,Taotao Peng,Ying Li,Chunshan Gui
Cypate, a heptamethine cyanine dye, is a prototypic near-infrared (NIR) theranostic agent for optical imaging and photothermal therapy. In the present study, a selective, sensitive, and rapid liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the quantitation of cypate in mouse plasma. The chromatographic separation was achieved using a short C 18 column (2.1 mm × 50 mm, 5 μm) with a run time of 5 min. The MS was operated in multiple reaction monitoring (MRM) mode via positive electrospray ionization. The ion transitions for cypate and internal standard IR-820 were m / z 626.3 → 596.3 and m / z 827.4 → 330.2, respectively. The method was linear over a concentration range of 1.0–500 ng/mL. The within-run and between-run precision was less than 14.4% with accuracy in the range of −13.4% ∼ 9.8%. The validated method was successfully applied to a pharmacokinetic study of cypate in mice following intravenous administration.
✓ 已验证
产品关联
DOI
PubMed
高影响因子
EUROPEAN JOURNAL OF MASS SPECTROMETRY
·
2019
·
IF 0.851
Shencong Lv,Henghui Wang,Yong Yan,Miaohua Ge,Jian Guan
A simple, rapid, and efficient liquid chromatography tandem mass spectrometry (LC–MS/MS) method, operated in electrospray ionization and quadrupole linear ion trap modes, has been developed for the identification and structural characterization of aflatoxins in peanuts and its derivative products or bean sauce. Samples (5 g) were extracted with acetonitrile/water/formic acid (79:20:1, v/v). After centrifugation and dilution, the extracts were separated on a C18 analytical column by gradient elution (acetonitrile/0.2% formic acid) and analyzed by UPLC–MS/MS. External calibration was used for qualification. The developed multiple reaction monitoring–information-dependent acquisition–enhanced product ion method enabled quantification and confirmation of the analytes in a single run. Enhanced product ion mode was used for qualitative analysis, while multiple reaction monitoring mode was used for quantitative analysis. An in-house library was constructed for identification. Calibration curves showed good linearity with correlation coefficients (r) higher than 0.994. Limits of detection were determined to be below 0.26 µg kg−1 for most analytes. The recoveries for those substances were in the acceptable range of 80.2%–119.1%. A new LC–MS3 method was established for further confirmation. One pickled pepper peanut was found to contain aflatoxins B1, B2, and G1 with contents of 90.93, 26.64, and 1.92 µg kg−1, respectively.
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2019
·
IF 2.813
Tengfei Li,Bin Huang,Duo Li,Yantong Zhu,Li Ding,Chang Shu
In this work, we developed and validated the specific, sensitive and simple LC–MS/MS method for quantification of eslicarbazepine in human plasma. The analyte samples were prepared through a simple one-step protein precipitation method by acetonitrile . The chromatographic separation was operated on an economical Hanbon ODS-2 C18 column (150 mm × 2.1 mm, 10 μm) with isocratic elution using 10 mM ammonium acetate containing 0.01% formic acid and acetonitrile (72:28, v/v) as the mobile phase at the flow rate of 0.5 mL/min. The mass quantification was carried on the multiple reaction monitoring (MRM) of the transitions of m / z 255.1 → 194.1 for eslicarbazepine and m / z 446.1 → 321.1 for glipizide (the internal standard), respectively. The established method was validated with acceptable specificity, linearity, accuracy, precision, extraction recovery, matrix effect and stability in accordance with FDA regulations. At last, the validated method was successfully applied to determination of eslicarbazepine in human plasma obtained from clinical study.
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2018
·
IF 2.831
Renjie Hui,Yueying Gao,Jingyi Liu,Haili Liu,Chunlei Tang,Bainian Feng
Heart failure (HF) is one of the most serious health problems worldwide. A new positive inotropic compound, an isonicotinylhydrazide derivative (AF-HF001) was designed recently. A liquid chromatography-tandem mass spectrometry (LC–MS/MS) method was developed for the determination of the target analyte in mouse plasma. Samples were prepared by one step precipitation with ethyl acetate and stored in acetonitrile. Chromatographic analysis was carried out on a Hypersil Gold C 18 column (2.1 mm × 50 mm, 3 μm) with a gradient mobile phase consisting of acetonitrile and 0.1% aqueous formic acid. The analyte was detected by selective reaction monitoring (SRM) mode with target quantitative ion pair of m/z 292.1 → 148.2, using praziquantel as the internal standard (IS) m/z 313.1 → 203.2. Good linearity ( r = 0.995) was observed over a wide concentration range. The validation of method showed acceptable recovery and precision. The method has been then applied to a very first pharmacokinetic assay of AF-HF001 in mice.
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2021
·
IF 3.935
Xinying He,Han Cao,Xia Li,Yan Li,Yunqiu Yu
Lysophosphatidylcholine (LPC) was commonly known as a class of significant differential metabolites of high relevance with many diseases including psoriasis, of which the accurate determination is of great importance to diagnosis or prediction to many diseases. However, it is challenging and complicated because of the enormous biological sample complexity and impurities interference. In this study, we synthesized a magnetic nanocomposite MG@PD@TiO 2 and took advantage of the interactions of Lewis acid−base between the phosphate groups in LPCs and Ti ions on MG@PD@TiO 2 nanomaterials for selective separation and enrichment of LPCs from complex biological matrix. The solid-phase extraction sample pretreatment process by means of MG@PD@TiO 2 nanomaterials coupled with LC–MS/MS method was then applied to actual determination of six typical LPCs (LPC 10:0, 14:0, 16:0, 18:0, 18:1, 22:0) in human plasma. The extraction conditions were scientifically optimized by single-factor test (adsorbent amount, adsorption and desorption time, elution solvent type, eluant volume). Under the optimal conditions, the detection limits (LOD, S/N = 3) and quantification limits (LOQ, S/N = 10) were 1 and 5 ng/mL for LPC 10:0 and LPC 14:0, 0.02 and 0.1 ng/mL for LPC 16:0 and LPC 18:1, 0.05 and 0.2 ng/mL LPC 18:0 and LPC 22:0, respectively. The intra- and inter-day precisions were 3.82–12.60 % (n = 6) and 3.29–13.50 % (n = 6) respectively, the recoveries were in the range of 91.92–113.69 % and the stability of the analytes in the matrix performed well with RSDs≤15.51 %. Finally, the developed method was successfully applied to the accurate determination of six LPCs biomarkers of plasma in patients with psoriasis (n = 10) and control groups (n = 10).
✓ 已验证
产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）