JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2025
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IF 3.1
Xiaoqian Chen,Luyao Yu,Yingxia Guo,Jiansong You,Meiyun Shi,Yalin Xi,Lei Yin
An analytical assay based on ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) technique for absolute quantification of vancomycin in complexed biological matrix was developed in this study. Reversed phase column with gradient elution was chosen for chromatographic separation of vancomycin and internal standard (IS) norancomycin. Sample pretreatment was performed by micro-solid phase extraction (μ-SPE) with Oasis® MAX μElution Plate (I.D., 30 μm). Multiple reaction monitoring (MRM) transition was chosen for monitoring of the analytes. For vancomycin, mass-to-charge ratio ( m/z ) of the MRM transition was 725.3→144.1; For norvancomycin, m/z of the MRM transition was 718.3→144.2. The running time was 3 minutes for each sample. The UHPLC-MS/MS method showed a good linear relationship (R 2 ≥0.995) in the concentration range of 0.5–100 μg/mL. The intra- and inter-day accuracies (relative error, RE) are within the range of −3.44 %-1.50 % and precisions are between 3.48 % and 10.19 %. μ-SPE could enrich the analytes and decrease the endogenous interferences, thereby improving the selectivity and sensitivity of the method. The analytical assay is selective, accurate and reproducible. The assay was successfully applied to therapeutic drug monitoring of vancomycin in clinical application.
研究领域:
临床医学
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分析化学
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DOI
PubMed
高影响因子
Food Analytical Methods
·
2023
·Vol. 16
·期 4
·689-698
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IF 2.9
Chu Qiqi,Wu Xinze,Chen Huaixia,Dang Xueping,Liu Xiaolan
A Cu 7 Zn 2 cluster functionalized copolymer monolithic column was prepared and applied as the adsorbent of pipette tip micro-solid phase microextraction of eight phthalate esters (PAEs). The physical morphology, chemical composition, thermal stability, and specific surface area of the monolithic column were characterized by scanning electron microscopy, Fourier-transform infrared spectroscopy, thermogravimetric analysis, and N 2 adsorption and desorption experiment. Cu 7 Zn 2 cluster acted as the adsorption site effectively improved the adsorption selectivity and capacity of the copolymer monolith for PAEs. The adsorption mechanism of Cu 7 Zn 2 copolymer monolith for 8 PAEs was deduced to be mainly the H-bond interaction. And, the chemical doping and copolymerization of Cu 7 Zn 2 cluster made the composite monolithic column more stable with a long service life. Under the optimized extraction conditions, a micro-solid phase extraction-high performance liquid chromatography method with ultraviolet detector (μ-SPE-HPLC-UV) was developed for the determination of 8 PAEs in edible oil. Wide linear ranges of 0.5–1000 μg/kg with correlation coefficients ( R 2 ) above 0.996 were obtained. The limits of detection (LODs) were in the range of 0.1–0.9 μg/kg. The proposed method was applied for the detection of 8 PAEs in edible oil with satisfactory recoveries between 83.5~100.2%, and the relative standard deviations were less than 8.1%. The results indicated that the Cu 7 Zn 2 functionalized copolymerized monolithic column was an ideal enrichment medium for the detection of PAEs in complex samples.
研究领域:
分析化学
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环境科学
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材料科学
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DOI
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
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2025
·
IF 3.8
Yu Luyao,Liu Meichen,Niu Ziyi,Zhang Jiarui,Deng Yue,Zhou Xinyue,You Jiansong,Xue Hongyu,Yin Lei,Shi Meiyun
Monodisperse polyethylene glycol (PEG) derivatives offer significant advantages over conventional polydisperse PEGs for biomedical applications due to their precisely defined molecular structures. This study establishes an eco-efficient, selective, and sensitive analytical assay integrating microscale solid-phase extraction (μ-SPE) with ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) to investigate the cellular uptake of HO-PEG 8 -OH polymers in MCF-7 cells. The method achieved greater than 91% recovery from 20 μL lysates using M-PEG 6 -OH as the internal standard, with validated linearity (10–1000 ng/mL, R > 0.997), accuracy (relative error < ± 7.49%), and precision (RSD < 7.50%). The novelty of the assay is the harmonization of analytical performance with green analytical chemistry principles. The validated method provides a robust platform for studying monodisperse PEG derivatives while addressing growing demands for sustainable analytical technologies. Green analytical chemistry metric assessments confirmed the environmental sustainability of the method. Cellular pharmacokinetic analysis revealed time-/concentration-dependent uptake kinetics of HO-PEG 8 -OH polymers in MCF-7 cells, showing 3.2-fold accumulation between 0.5 and 48 h exposure. These findings offer important insights for PEG-based drug delivery system optimization and establish a new standard for environmentally conscious bioanalytical method development. Graphical
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高影响因子
MICROCHEMICAL JOURNAL
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2018
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IF 2.746
Guihua Gao,Yanyan Xing,Tingting Liu,Jian Wang,Xiaohong Hou
Four water stable metal-organic frameworks (MOFs), MIL-101(Cr), MIL-100(Fe), MIL-53(Al), and UiO-66(Zr), were used as adsorbents for concentration of four androgens and progestogens from water. The adsorption abilities of target analytes on the four MOFs were investigated by experimental and molecular simulation strategies, and UiO-66(Zr) was ultimately selected as the sorbent to develop a porous membrane protected micro-solid-phase extraction (μ-SPE) method for simultaneous extraction androgens and progestogens in environmental water samples followed by LC-MS/MS detection. Several variables affecting the extraction efficiency were systematically investigated, including pH, salt concentration, extraction time, kind of desorption solvent, and desorption time. Under the optimized conditions, excellent linearity was obtained in the range of 20.32–2032 ng/L for T, 10.24–1024 ng/L for P, 7.624–762.4 ng/L for TP , and 8.376–837.6 ng/L for MPA . Limits of detection (LODs) and limits of quantification (LOQs) were 10 ng/L and 20 ng/L for T, 4.0 ng/L and 10 ng/L for P, 2.0 ng/L and 7.0 ng/L for TP, and 3.0 ng/L and 8.0 ng/L for MPA, respectively. The recoveries were ranged from 80.5% to 102.4%. Furthermore, the μ-SPE device could be used for at least 10 extractions (RSD < 10.0%). Meanwhile, comparison was made with solid-phase extraction, and the developed method was demonstrated to be a convenient and eco-friendly pretreatment method for water samples.
研究领域:
环境科学
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分析化学
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材料科学
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高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
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2019
·Vol. 411
·期 18
·4073-4084
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IF 3.286
Xia Ling,He Yuanyuan,Xiao Xiaohua,Li Gongke
Herein, a total online device based on field-assisted extraction (FAE), micro-solid-phase extraction (μ-SPE), and high-performance liquid chromatography (HPLC) was designed. Solid samples were pretreated with ultrasound-microwave synergic effects, and then the extract was cleaned up online with a monolithic column, followed by HPLC analysis. The cross-actions between ultrasound and microwave along with other extraction parameters were studied systematically. The efficiency of this online method was verified in the determination of polycyclic aromatic hydrocarbons (PAHs) in foods and tetracycline antibiotics (TCAs) in cosmetic samples. The detection limits of nine PAHs including fluorene, phenanthrene, anthracene, fluoranthene, benzo[k]fluoranthene, benz[a]anthracene, benzo[b]fluoranthene, pyrene, and benzo[a]pyrene were all within 0.075–0.30 μg/kg, as well as four TCAs including oxytetracycline, tetracycline, chlortetracycline, and doxycycline were within 0.02–0.06 μg/kg. Six PAHs were found in roast potatoes and baked fish and the recoveries were in the range of 71.5–119.7% with RSDs of 0.2–10.9% ( n = 3). The recoveries for TCAs in cosmetic samples were in the range of 75.3–118.0% with RSDs lower than 8.2% ( n = 3). Compared with those offline methods, this total online FAE-μ-SPE-HPLC method not only simplifies the operation process, but also increases the precision and accuracy. Beyond trace analytes analysis in solid and semi-solid matrixes, application of this total online analysis method can also be extended to investigate field-assisted extraction mechanisms.
Graphical abstract
研究领域:
分析化学
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环境科学
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药物分析
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PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2026
·
IF 4.1
Zhou Xinyue,Duan Sufei,Lou Yuye,Deng Yue,Feng Shuang,Liu Jiale,Zhang Jiarui,Xi Yalin,Shi Meiyun,Yin Lei
A sensitive UPLC-MS/MS method was developed and validated for quantifying polyethylene glycol 1000 (PEG1000) in zebrafish tissues, featuring a systematic comparison of two MS acquisition strategies. Through comprehensive optimization, the ammonium adduct [M+NH 4 ] + of the representative 18-EO oligomer ( m/z 828.5) was selected as the precursor ion, achieving approximately fourfold higher signal intensity than [M+H] + . Critically, the conventional high declustering potential in-source CID approach monitoring fragment ions was outperformed by the optimized MRM method monitoring the intact ammoniated precursor, which demonstrated 2.7-fold signal enhancement and superior selectivity. The integration of micro-solid-phase extraction (μ-SPE) further improved method performance, yielding 1.5-fold signal gain and markedly reduced matrix effects compared to conventional protein precipitation. The fully validated method exhibited excellent linearity (0.5–50 μg/mL, r > 0.995), accuracy, precision, and stability. Application to zebrafish tissue distribution studies revealed pronounced organ-specific accumulation following aqueous exposure to 200 μg/mL PEG1000, with highest concentrations in intestine tissue exhibiting a time-dependent increase, followed by muscle, while muscle maintained consistently low levels. This analytical platform, synergistically combining μ-SPE cleanup and ammoniated adduct-based MRM, offers superior sensitivity over in-source CID approaches and provides a practical framework for polymer bioanalysis, yielding critical insights into the in vivo fate of PEG-based compounds. The key novelties of this work are the following: (i) the first systematic comparison between ammoniated adduct MRM and high-DP in-source CID for PEG1000 quantification; (ii) the introduction of μ-SPE for sample preparation in zebrafish tissues, achieving 1.5-fold signal enhancement; and (iii) the successful application of this platform to reveal organ-specific accumulation patterns of PEG1000. Graphical abstract
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高影响因子
危险品化学品经营许可证（带存储）