JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2017
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IF 3.255
Katerina Grigori,Yannis L. Loukas,Anđelija Malenović,Vicky Samara,Anastasia Kalaskani,Efi Dimovasili,Magda Kalovidouri,Yannis Dotsikas
A sensitive Liquid Chromatography tandem mass spectrometry (LC–MS/MS) method was developed and validated for the quantitative analysis of three potential genotoxic impurities (318BP, M9, S5) in meropenem Active Pharmaceutical Ingredient (API). Due to the requirement for LOD values in ppb range, a high concentration of meropenem API (30 mg/mL) had to be injected. Therefore, efficient determination of meropenem from its impurities became a critical aim of this study, in order to divert meropenem to waste, via a switching valve. After the selection of the important factors affecting analytes’ elution, a Box-Behnken design was utilized to set the plan of experiments conducted with UV detector. As responses, the separation factor s between the last eluting impurity and meropenem, as well as meropenem retention factor k were used. Grid point search methodology was implemented aiming to obtain the optimal conditions that simultaneously comply to the conflicted criteria. Optimal mobile phase consisted of ACN, methanol and 0.09% HCOOH at a ratio 71/3.5/15.5 v/v. All impurities and internal standard omeprazole were eluted before 7.5 min and at 8.0 min the eluents were directed to waste. The protocol was transferred to LC–MS/MS and validated according to ICH guidelines.
研究领域:
分析化学
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药物分析
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药学
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JOURNAL OF ETHNOPHARMACOLOGY
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2026
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IF 6.8
Hongrui Ma,Xin Ding,Junli Liang,Ping Li,Runuo Wang,Ya Zhang,Guangguo Tan
Ethnopharmacological relevance Aconiti Lateralis Radix Praeparata (Fuzi in Chinese) is an herbal medicine for restoring yang from collapse. However, the multiregional neurotoxicity of Fuzi was unclear. Aim of the study This work was designed to discover the multiregional neurotoxicity-associated metabolic alterations induced by Fuzi in brain of rat. Materials and methods Fuzi-distributed components in cerebrospinal fluid and multiple brain regions were analyzed by using ultra-high performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry (UHPLC-QTOF-MS). The multiregional neurotoxicity including hippocampus, striatum and cerebellum was evaluated by behavioral tests, biochemical examinations, Hematoxylin/eosin (H&E), Nissl staining, TUNEL staining, reactive oxygen species and metabolomic analyses. Both cerebrospinal fluid metabolomics and the multiregional target tissue (hippocampus, striatum and cerebellum) metabolomics of the brain, based on UHPLC-QTOF-MS, were conducted to reveal the metabolic changes associated with Fuzi neurotoxicity. Results 13, 11, 11 and 8 ingredients of Fuzi were distributed into the cerebrospinal fluid, hippocampus, striatum, and cerebellum, respectively. Fuzi exposure could cause motor dysfunction and anxiety-like behaviors and decrease the level of brain derived neurotrophic factor (BDNF) and increase the level of neuron specific enolase (NSE). Fuzi exposure produced oxidative stress, neuronal lesions, neuronal apoptosis and metabolic alterations, which produced the multiregional neurotoxicity in the brain. The differentially expressed metabolites associated with Fuzi exposure in the cerebrospinal fluid, hippocampus, striatum and cerebellum predominantly involved glycerophospholipid metabolism, sphingomyelin metabolism, arachidonic acid metabolism, purine metabolism, amino acid metabolism, TCA cycle and fatty acid β-oxidation. Conclusion Fuzi exposure produced the multiregional neurotoxicity in the hippocampus, striatum and cerebellum of the brain.
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TALANTA
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2026
·
IF 6.7
Feng Chen,Ziwei Deng,Yueping Jiang,Yayun Tan,Xiaoxia Yang,Huanhuan Li,Wendan Zhang,Xiangjin Shu,Aimin Wang,Chengfeng Qiu
Therapeutic drug monitoring (TDM) is essential for optimizing antimicrobial therapy and curbing resistance, yet conventional venipuncture limits its widespread application due to invasiveness and operational complexity. This study aimed to establish a rapid LC-MS/MS method for simultaneous quantification of 12 antimicrobial agents and to evaluate the feasibility of using fingertip capillary serum as an alternative to venous serum for TDM. A liquid chromatography tandem mass spectrometry method was developed and validated for the simultaneous quantification of vancomycin, linezolid, voriconazole, sulfamethoxazole, trimethoprim, piperacillin, cefoperazone, ceftazidime, ceftobiprole, meropenem, imipenem, and cilastatin in human serum. The method was applied to analyze 379 paired clinical samples (fingertip serum versus venous serum), and agreement between the two sampling approaches was assessed using Deming regression and Bland Altman analysis. The method required only 10 μL of serum and a total run time of 4 min. Deming regression slopes ranged from 0.910 to 1.017. Bland Altman analysis showed that 100.0% of the data points fell within ±20.0% limits of agreement for all antibiotics except vancomycin (96.7%) and cilastatin (97.5%). This study provides large scale clinical evidence demonstrating high concordance between fingertip serum and venous serum concentrations for 12 antimicrobial agents. By directly obtaining serum, this approach fundamentally avoids the hematocrit effect and matrix conversion issues inherent in whole blood microsampling, offering a minimally invasive TDM strategy fully aligned with the gold standard matrix. This strategy is particularly suitable for special populations such as children, the elderly, and critically ill patients.
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JOURNAL OF CHROMATOGRAPHY A
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2026
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IF 4
Jinlin He,Luying Shen,Dunming Xu,Ting Sun,Yan Chen,Jinsheng Hu,Yan Ji,Lijuan Yan
First demonstration of C18-column HILIC-like separation for aminoglycosides. • Hydrophilic retention via water layer & vicinal silanols on base-deactivated silica. • Tandem WCX-C18 SPE protocol developed for effective matrix cleanup. • Robust, MS-compatible, practical monitoring of aminoglycoside residues in foods. An LC–MS/MS method was developed for the simultaneous determination of 16 aminoglycosides (AGs) in pork, chicken, milk, and eggs using a conventional Hypersil base-deactivated silica (BDS) C 18 column operated under HILIC-like conditions. Unlike typical C 18 -based methods that rely on ion-pairing reagents in the LC mobile phase, separation was achieved with an ion-pair-free mobile phase consisting only of 0.1% formic acid and acetonitrile under gradient elution. Column comparison, aqueous-fraction experiments, and SRM 870 probe testing indicated a mixed retention mechanism involving hydrophilic partitioning into a water-enriched interfacial layer and reversible interactions with accessible residual silanol sites. Because the method prioritizes MS compatibility and reproducible multi-residue quantification, compound-specific MRM transitions and matrix-matched calibration were used to ensure selectivity and quantitative reliability. The method showed good linearity (R² > 0.99), satisfactory accuracy (71.2–99.8%) with reported standard deviations, acceptable precision (CV ≤ 11.3%), and low detection limits (LODs 3–15 μg/kg; LOQs 10–50 μg/kg). Overall, this work demonstrates that a conventional C 18 column can exhibit pronounced hydrophilic selectivity under high-organic conditions, offering a practical, MS-friendly alternative for aminoglycoside residue analysis and informing future stationary-phase development for hydrophilic separations.
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MICROCHEMICAL JOURNAL
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2025
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IF 5.1
Mengmeng Feng,Huifang Ge,Ting Zhang,Jingbo Liu,Boqun Liu,Yali Yu
The quantification and analysis of free amino acids (FAAs) in serum is important for illness diagnosis due to its content varies with the body’s condition. In this study, a new sensitive analytical method based on liquid chromatography electrospray ionization mass spectrometry (LC-ESI-MS/MS) was optimized for simple and rapid simultaneous detection of 20 amino acids by pre-column derivatization. Amino acid derivatized by 9-fluorenyl methyl chloroformate (FMOC-Cl) were eluted and separated by simple mobile phase reagent in 20 min via gradient elution using a traditional reverse phase C18 column (150 × 4.6 mm, 5 μm), at the flow rate of 0.8 mL/min. After optimizing derivatization, LC-MS/MS conditions, and sample pre-treatment, this method was verified with LODs and LOQs ranging from 0.0237 to 0.2391 ng/mL and 0.079 to 0.7971 ng/mL. The intra- and inter-day precision was no more than 10 %. The overall accuracy and recovery varied from 88.4-111 % and 88.7–114 %, respectively. Those methods were first applied to mice serum with ulcerative colitis. The results showed that the levels of Ala, Arg, Trp, Lys, Cys, Tyr, and Phe significantly increased in pre-treated group by egg white peptides, which will participate in metabolism. This study provides a valuable reference for further research on the pathogenesis of ulcerous colitis and the development of functional foods to relieve inflammation and balance metabolism.
研究领域:
分析化学
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医学
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营养学
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FOOD CHEMISTRY
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2025
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IF 9.8
Luyue Zhao,Shu Li,Tong Wang,Sinan Wang,Jinhua Zhan,Jing Chen
Perfluorinated compounds are of extensive concern due to their prevalent use, persistence, and toxicities. There is a demand for extraction adsorbents that are efficient, easy to synthesize, and cost-effective. Herein, a magnetic nylon 6 nanocomposite (M-Ny6) was synthesized through a simple process and utilized as an adsorbent in magnetic solid-phase extraction (MSPE) of perfluorooctanoic acid (PFOA). The MSPE condition was optimized and the adsorption characteristics for PFOA was investigated. Based on the interaction between the amide groups on M-Ny6 and PFOA, the MSPE method was coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS) for analyzing trace levels of PFOA in environmental water and bottled beverages. The established method demonstrated a detection limit of 1.2 ng L −1 with linear range across 50–800 ng L −1 and satisfactory recoveries (82.3–113.0 %) in spiked samples. The experimental results indicated that M-Ny6 is a promising and cost-effective MSPE adsorbent offering potential for large-scale applications in food analysis.
研究领域:
环境科学
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分析化学
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高影响因子
MOLECULES
·
2024
·Vol. 29
·期 5
·1037
·
IF 4.2
Yujie Zhang,Jingjie Cao,Jiahan Su,Tingting He,Qianru Wang,Feng Wei,Xin Guo,Qibing Mei,Jing Zeng
Bitespiramycin, has been shown to have a therapeutic effect against respiratory tract inflammation, including a potential effect against COVID-19. A current clinical trial in China showed that bitespiramycin was an effective treatment for severe pneumonia and intracranial infection. However, there is lack of an analytical method to elucidate the distribution of bitespiramycin. In this study, a highly sensitive, rapid and reliable UPLC–MS/MS method was developed to comprehensively characterize the bitespiramycin distribution in various bio-samples, which is significantly improved upon the published work. A rapid sample preparation method was developed by usingn-butanol as the solvent to extract bitespiramycin from different bio-samples. The extract was then directly analyzed by UPLC–MS/MS coupled with an alkaline-resistant column after centrifugation which avoids the time-consuming concentration process under nitrogen and redissolution. The method was employed to accurately quantify bitespiramycin and its metabolites in rat plasma, tissues, and human cerebrospinal fluid. Notably, the presence of bitespiramycin and its metabolites was identified for the first time in various rat organs including brain, testis, bladder and prostate as well as in human cerebrospinal fluid. This newly developed approach shows great promise for drug distribution assays including other antibiotics and can help elucidate the ADME of bitespiramycin.
研究领域:
药理学
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分析化学
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临床研究
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药物开发
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Scientific Reports
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2017
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IF 4.259
Cong Xie,Tong-Meng Yan,Jia-Mei Chen,Xiao-Yan Li,Juan Zou,Li-Jun Zhu,Lin-Lin Lu,Ying Wang,Fu-Yuan Zhou,Zhong-Qiu Liu,Ming Hu
This study aims to determine whether enzyme activities are correlated with protein amounts and mRNA expression levels of five major human sulfotransferase (SULT) enzymes in 10 matched pericarcinomatous and hepatocellular carcinoma liver samples. The MRM UHPLC-MS/MS method, Western blot and RT-PCR were used along with SULT activity measurement using probe substrates. The LC-MS/MS method was specific for all five tested SULTs, whereas Western blot was specific for only two isoforms. The activities of SULT1A1, SULT1B1, SULT1E1 and SULT2A1 in 9 of 10 samples showed a significant decrease in tumor tissues relative to matched pericarcinomatous tissues, whereas the activities of SULT1A3 in 7 of 10 samples increased. The turnover numbers of SULTs did not change, except for SULT1A1. A generally high degree of correlations was observed between SULT activities and protein amounts (r 2 ≥ 0.59 except one), whereas a low degree of correlations was observed between SULT activities and mRNA expression levels (r 2 ≤ 0.48 except one). HCC reduced the SULT activities via impaired protein amounts. LC-MS/MS quantification of SULTs is highly reliable measurement of SULT activities, and may be adopted for implementing precision medicine with respect to drugs mainly metabolized by SULTs in healthy and HCC patients.
研究领域:
药理学
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分子生物学
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肿瘤学
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临床化学
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FOOD RESEARCH INTERNATIONAL
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2026
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IF 8.8
Mengyao Zhang,Tianyi Tao,Zixuan Wang,Shijie Ding,Guanghong Zhou,Chong Wang
Cultured meat presents significant potential as a sustainable supplement to traditional livestock farming. Addressing the critical challenge of residual chemical substances from the culture media, this study established a rapid method combining protein precipitation (PP) with liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the quantitative analysis of 12 risk substances in both porcine cultured meat biomass and washing solutions. All validation parameters, including linearity, sensitivity, precision, accuracy, recovery, matrix effect, dilution integrity and stability, met the predefined acceptance criteria. The results demonstrated that consecutive centrifugal washing cycles significantly reduced residue levels in porcine cultured meat biomass, with the majority of the 12 target substances effectively removed after four cycles. Analysis of 15 production batches revealed that 9 out of the 12 target substances were below the limit of detection (LOD) in the final product. For the remaining three substances, the mean concentrations were 307.91 μg/kg for forskolin, 568.04 μg/kg for thymidine, and 397.61 μg/kg for N -acetylcysteine. A target hazard quotient (THQ) assessment confirmed that none of the 12 residues posed a health risk. These findings provide the technical groundwork and theoretical rationale needed to optimize quality and safety specifications in the cultured meat industry.
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2015
·Vol. 407
·期 24
·7359-7368
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IF 3.436
Zhao Zhiyong,Liu Na,Yang Lingchen,Deng Yifeng,Wang Jianhua,Song Suquan,Lin Shanhai,Wu Aibo,Zhou Zhenlei,Hou Jiafa
Mycotoxins have the potential to enter the human food chain through carry-over of contaminants from feed into animal-derived products. The objective of the study was to develop a reliable and sensitive method for the analysis of 30 mycotoxins in animal feed and animal-derived food (meat, edible animal tissues, and milk) using liquid chromatography–tandem mass spectrometry (LC–MS/MS). In the study, three extraction procedures, as well as various cleanup procedures, were evaluated to select the most suitable sample preparation procedure for different sample matrices. In addition, timed and highly selective reaction monitoring on LC–MS/MS was used to filter out isobaric matrix interferences. The performance characteristics (linearity, sensitivity, recovery, precision, and specificity) of the method were determined according to Commission Decision 2002/657/EC and 401/2006/EC. The established method was successfully applied to screening of mycotoxins in animal feed and animal-derived food. The results indicated that mycotoxin contamination in feed directly influenced the presence of mycotoxin in animal-derived food.
Multi-mycotoxin analysis of animal feed and animal-derived food using LC-MS/MS
研究领域:
食品安全
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分析化学
·
毒理学
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2023
·
IF 3
Peng Qi,Ping Li,Lijiao Qiao,Huaqian Xue,Yanni Ma,Shijie Wei,Xiaoying Yang,Hao Zhang,Yuxin Zhang,Yifan Wang,Shaolong He,Hongfeng Quan,Wenping Zhang
Pirarubicin (THP), doxorubicin (DOX), cyclophosphamide (CTX), and vincristine (VCR) are widely used in the treatment of patients with non-Hodgkin's Lymphoma. Herein, a precise and sensitive method was developed for the determination of THP, DOX, CTX and VCR in human plasma by high-performance liquid-chromatography–tandem mass spectrometry (LC-MS/MS). Liquid-liquid extraction was applied to extract THP, DOX, CTX, VCR, and the internal standard (IS, Pioglitazone) in plasma. Agilent Eclipse XDB-C18 (3.0 mm × 100 mm) was utilized and chromatographic separation was obtained in eight minutes. Mobile phases were composed of methanol and buffer (10 mM ammonium formate containing 0.1% formic acid). The method was linear within the concentration range of 1–500 ng/mL for THP, 2–1000 ng/mL for DOX, 2.5–1250 ng/mL for CTX, and 3–1500 ng/mL for VCR. The intra- and inter-day precisions of QC samples were found to be below 9.31 and 13.66%, and accuracy ranged from −0.2 to 9.07%, respectively. THP, DOX, CTX, VCR and the internal standard were stable in several conditions. Finally, this method was successfully utilized to simultaneously determine THP, DOX, CTX and VCR in human plasma of 15 patients with non-Hodgkin's Lymphoma after intravenous administration. Finally, the method was successfully employed in the clinical determination of THP, DOX, CTX, and VCR in patients with non-Hodgkin lymphoma after administration of RCHOP (rituximab plus cyclophosphamide, doxorubicin, vincristine, and prednisone) regimens.
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MOLECULES
·
2023
·Vol. 28
·期 5
·2377
·
IF 4.6
Zili Guo,Bianbian Gao,Miaoliang Fan,Lisha Chen,Changjun Zhang,Xianrui Liang,Weike Su,Yuanyuan Xie
XYY-CP1106, a candidate compound synthesized from a hybrid of hydroxypyridinone and coumarin, has been shown to be remarkably effective in treating Alzheimer’s disease. A simple, rapid and accurate high-performance liquid chromatography coupled with the triple quadrupole mass spectrometer (LC-MS/MS) method was established in this study to elucidate the pharmacokinetics of XYY-CP1106 after oral and intravenous administration in rats. XYY-CP1106 was shown to be rapidly absorbed into the blood (Tmax, 0.57–0.93 h) and then eliminated slowly (T1/2, 8.26–10.06 h). Oral bioavailability of XYY-CP1106 was (10.70 ± 1.72)%. XYY-CP1106 could pass through the blood–brain barrier with a high content of (500.52 ± 260.12) ng/g at 2 h in brain tissue. The excretion results showed that XYY-CP1106 was mainly excreted through feces, with an average total excretion rate of (31.14 ± 0.05)% in 72 h. In conclusion, the absorption, distribution and excretion of XYY-CP1106 in rats provided a theoretical basis for subsequent preclinical studies.Keywords:XYY-CP1106;Alzheimer’s disease;LC-MS/MS;pharmacokinetics;tissue distribution;excretion study
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