TALANTA
·
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
·
2026
·
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
·
2025
·
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
·
医学
·
营养学
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FOOD CHEMISTRY
·
2025
·
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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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
·
药物开发
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Scientific Reports
·
2017
·
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
·
分子生物学
·
肿瘤学
·
临床化学
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FOOD RESEARCH INTERNATIONAL
·
2026
·
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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JOURNAL OF SEPARATION SCIENCE
·
2019
·Vol. 42
·期 20
·3234-3242
·
IF 2.516
Zi-Ling Li,Na Li,Li Du,Ya-Hui Wang,Bo Fang,Man-Man Wang,Qian Wang
The biomonitoring of hydroxy polycyclic aromatic hydrocarbons in urine, as a direct way to access multiple exposures to polycyclic aromatic hydrocarbons, has raised great concerns due to their increasing hazardous health effects on humans. Solid-phase extraction is an effective and useful technique to preconcentrate trace analytes from biological samples. Here, we report a novel solid-phase extraction method using a graphene oxide incorporated monolithic syringe for the determination of six hydroxy polycyclic aromatic hydrocarbons in urine coupled with liquid chromatography-tandem mass spectrometry. The effect of graphene oxide amount, washing solvent, eluting solvent, and its volume on the extraction performance were investigated. The fabricated monoliths gave higher adsorption efficiency and capacity than the neat polymer monolith and commercial C 18 sorbent. Under the optimum conditions, the developed method provided the detection limits ( S/N = 3) of 0.02–0.1 ng/mL and the linear ranges of 0.1–1500 ng/mL for six analytes in urine sample. The recoveries at three spiked levels ranged from 77.5 to 97.1%. Besides, the intra column-to-column ( n = 3) and inter batch-to-batch ( n = 3) precisions were ≤ 9.8%. The developed method was successfully applied for the determination of hydroxy polycyclic aromatic hydrocarbons in urine samples of coke oven workers.
研究领域:
分析化学
·
环境健康科学
·
毒理学
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2019
·
IF 2.813
Lizhi Zhao,Zhou Li,Zhen Zhou,Xiuyuan Kang,Baihuan Fang,Huan Ma,Qinghua Ge
An ultra performance liquid chromatography-tandem mass spectrometric (UHPLC-MS/MS) method has been developed for the simultaneous determination of tenofovir alafenamide (TAF) and it's metabolite tenofovir (TFV) in human plasma. The analytes and inter standards, TAF-d5 and TFV-d6 were extracted from human plasma via protein precipitation (PPT) and only 200 μl plasma was needed. Chromatography separation was achieved on a Waters Acquity UHPLC HSS T3 column (100 * 2.1 mm, 1.8 μm) with a total run time of 10 min. A tandem mass spectrometric detection was conducted using multiple reaction monitoring (MRM) mode under positive ionization mode with an electrospray ionization (ESI) interface. The method was developed and validated over the concentration range of 4.00–400 ng/ml for TAF and 0.400–40.0 ng/ml for TFV, respectively. Each analyte in acidified plasma was found stable during sample storage, preparation and analytical procedures. The method has successfully overcame the lack of stability of analytes in plasma samples and been applied to the pharmacokinetics study of treatment of 25 mg TAF in 8 healthy volunteers under fasting condition.
研究领域:
药物分析
·
临床药理学
·
分析化学
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2015
·Vol. 407
·期 24
·7359-7368
·
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
·
分析化学
·
毒理学
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CHROMATOGRAPHIA
·
2018
·Vol. 81
·期 12
·1673-1684
·
IF 1.401
Cheng Jie,Kong Xiaojian,Liu Shucheng,Che Dandan,Sun Zhiwei,Li Guoliang,Ping Meiling,Tang Jingpu,You Jinmao
A selective and accurate liquid chromatography–mass spectrometry (LC-MS) method based on magnetic solid-phase extraction (MSPE) and isotope-coded derivatization was developed and validated. The magnetic polydopamine (Fe 3 O 4 @PDA) was prepared as sorbent for enrichment of ten ultraviolet (UV) filters from domestic wastewater samples. The obtained extract and standards were labeled by a pair of isotope-coded derivatization reagents d 0 -/d 3 -10-methylacridone-2-sulfonyl chloride (d 0 -/d 3 -MASC), respectively. The quantification of UV filters was achieved by calculation of the peak area ratios of d 0 -MASC/d 3 -MASC-labeled derivatives. The isotope-coded derivatization strategy was confirmed to be effective in reducing matrix effect and improving sensitivity. Excellent linearity is established with the correlation coefficients > 0.9922. The limits of detection (LODs) were in the range of 0.056–0.128 µg L −1 , and the limits of quantitation (LOQs) were in the range of 0.193–0.315 µg L −1 . The developed method has been successfully applied to the quantification of UV filters in domestic wastewater samples with recoveries ranging from 95.6 to 103.6%. Graphical abstract
研究领域:
环境科学
·
分析化学
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
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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