TALANTA
·
2023
·
IF 6.1
Qing Chen,Yan Xu,Xueting Feng,Yuhan Xiang,Jiayue Ni,Guoyu Ding,Qunxiang Ren,Ming-sheng Zhou
The grafting of a drug molecule, i.e., geldanamycin (GA) onto polyethyleneimine (PEI)-coated magnetic nanoparticle produces a novel composite, GA@Fe 3 O 4 –NH 2 . The composite is confirmed by characterizations with FT-IR, Raman, SEM, EDS, VSM and TEM. Due to the high binding-affinity of GA with myosin heavy chain (MYH), GA@Fe 3 O 4 –NH 2 exhibits excellent adsorption performance towards myosin. Consequently, a solid-phase extraction procedure is established for highly efficient and selective separation of myosin from pig heart extract. At pH 6.0, an adsorption efficiency of 97.1 % is achieved for treating 100 μg mL −1 myosin (0.1 mL) with 0.1 mg GA@Fe 3 O 4 –NH 2 as adsorbent. The adsorption behavior of myosin onto GA@Fe 3 O 4 –NH 2 fits Langmuir model, corresponding to a theoretical adsorption capacity of 518.1 mg g −1 . The adsorbed myosin can be readily recycled by the SDS solution (1 %, m/m) with an elution efficiency of 91.8 %. According to circular dichroism spectroscopy, the conformational changes of myosin during adsorption and elution are reversible. For practical application, myosin is successfully isolated from the pig left ventricular protein extract with GA@Fe 3 O 4 –NH 2 , and SDS-PAGE and LC-MS/MS showed that myosin had high purity and a total of 716 proteins could be identified. Significantly, Geldamycin-encapsulated magnetic nanoparticle for the separation of myosin well exploits the potential of the nanomaterials modified by drug molecules in the separation and purification of target proteins.
研究领域:
蛋白质组学
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纳米技术
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生物医学工程
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分析化学
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PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2025
·
IF 4
Yang Yang,Jin Wang,Jia Qiu,Yan Luo,Chun Yang,Shali Tang,Hui Cao,Qian Wang,Xiaojing Lai
To monitor per- and polyfluoroalkyl substances (PFAS) in food contact materials (FCMs), an LC-MS/MS method for the simultaneous detection of 35 PFAS was developed and validated in paper and plastic products. Chromatographic and mass spectrometry parameters, extraction solvents, matrix effects in details were studied. The impact of matrix effects on PFAS concentration was analyzed, revealing that the matrix enhancement effect was more significant for some PFAS with low concentrations. In order to eliminate the matrix effect and enhance detection accuracy, a straightforward pretreatment method combining methanol ultrasonic extraction with dispersive solid-phase extraction (d-SPE) was established. PFHpA, PFDA, PFTriDA, PFTeDA, PF-3,7-DMOA, HFPO-DA, PFHxS, PFHpS, PFOS, 4:2 FTS, 6:2 FTS, 8:2 FTS, 10:2 FTS, and 6:2 diPAP required further d-SPE extraction with PSA, and other substances could be directly extracted by methanol ultrasonic treatment. The recoveries of the established method for all compounds ranged from 62.40 to 135.80%, with a relative standard deviation (RSD) of 0.15% to 16.81%. The limit of quantitation was between 0.005 and 0.02 mg·kg −1 . The method was applied to detect PFAS in 119 FCMs, resulting in the identification of 15 PFAS.
研究领域:
分析化学
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食品安全
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PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2025
·
IF 3.8
Li Wenya,Gao Bingling,Yang Tao,Tang Liping,Song Dan,Li Hongmei,Sun Keqi,Xiao Peng
3,3′,5-Triiodothyronine (T3) plays a crucial role in the diagnosis and evaluation of thyroid diseases. The current reference measurement procedure (RMP) has been in place for 20 years and is widely adopted by reference laboratories around the world. To enhance the performance of the RMP, we developed and validated a simplified, SI-traceable candidate RMP specifically targeting serum total T3 (TT3) using isotope dilution-liquid chromatography with tandem mass spectrometry (ID-LC–MS/MS). Specifically, T3 reference material was employed as the standard. Compared to the RMP, our method incorporates a simplified serum cleanup process involving protein precipitation and nitrogen drying. The method validation followed ISO guidelines for measurement uncertainty assessment. Our results indicated that there was no significant conversion of T4 into metabolites during the serum pretreatment. The lower limit of the measuring interval was determined to be 0.077 nmol/L, and the regression model was linear across a range of 0.016 to 13.086 nmol/L. The imprecision of intra-assays ranged from 0.1 to 1.9%, while inter-assay imprecision ranged from 0.5 to 1.2%. The bias observed when analyzing SRM971 was between − 0.34 and − 1.65%. This candidate RMP demonstrated excellent agreement with the RMPs developed by RELA activity, showing a mean bias falling within the educational mean ratio (6%). The measurement uncertainties were 0.022 nmol/L for RELA2023A and 0.120 nmol/L for RELA2023B. In conclusion, the developed candidate RMP is traceable, reliable, and easy to operate, showing promising potential for the development of serum reference materials and the standardization of routine assays. Graphical
研究领域:
临床检验学
·
内分泌学
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PubMed
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2019
·Vol. 42
·期 16
·2592-2601
·
IF 2.516
Hongmin Zhang,Xintong Hu,Miao Qiao,Yang Li,Shijie Cao,Liqin Ding,Xinchi Feng,Ning Kang,Deqin Zhang,Feng Qiu
A rapid and sensitive liquid chromatography with tandem mass spectrometry method was developed and validated for simultaneous determination of puerarin, daidzin, daidzein, 3′-hydroxy puerarin, and genistein in rat plasma after oral administration of Puerariae lobatae radix extract. The method of protein precipitation with acetonitrile was used for sample preparation. Chromatographic separation was achieved on a C 18 column with the mobile phases of acetonitrile/water containing 0.1% formic acid. The analytes were detected by mass spectrometer with an electrospray ionization source operating in the negative ion mode. The linearity, precision, accuracy, dilution reliability, recovery, matrix effects, and stability of the method were within acceptable ranges. The developed method was successfully used to compare the pharmacokinetic characteristics of five analytes in normal and type 2 diabetics rats after oral administration of Puerariae lobatae radix extract. Several pharmacokinetic alterations were observed and this might be caused by the pathological state of type 2 diabetes.
研究领域:
药理学
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分析化学
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糖尿病研究
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DOI
PubMed
高影响因子
FOOD RESEARCH INTERNATIONAL
·
2026
·
IF 8.8
Yuanyuan Zhao,Yongmao Lu,Tian Yang,Shaohua Hu,Yuanyuan Yan,Xingguo Wang,Wei Wei
Multi-method strategy enhances accuracy in human milk vitamin research. • Mass spectrometry achieved precise 25(OH)D₂/₃ quantification in human milk. • Immunoassays offered rapid screening but showed a 72.98% positive bias. • Liquid chromatography profiled vitamins A and E but lacked sensitivity for D and K. • 25(OH)D₃ increased slightly, while 25(OH)D₂ declined across lactational stages. Accurate analysis of vitamin D in human milk is essential for infant nutrition but remains analytically challenging due to low levels and a complex matrix. This study evaluates a practical multi-method strategy using LC-MS/MS, ELISA, and UPLC-PDA for vitamin D analysis in human milk. LC-MS/MS precisely quantified 25(OH)D₂ and 25(OH)D₃ with assay LOQ of 0.045 ng/mL and 0.100 ng/mL, respectively. ELISA showed a 11.58 ng/mL positive bias of vitamin D which limits use for accurate quantification. UPLC-PDA profiled vitamins A and E effectively but lacked sensitivity for vitamin D. Longitudinally, LC-MS/MS results show 25(OH)D₃ and total 25(OH)D concentrations remained relatively stable, with medians ranging from 0.141 to 0.281 ng/mL and 0.263 to 0.315 ng/mL, respectively, across the study period, while 25(OH)D₂ peaked at 8 weeks before declining. This study establishes LC-MS/MS as the preferred analytical strategy for quantifying 25(OH)D 2 and 25(OH)D 3 in human milk, providing critical data to assess infant nutritional intake and guide clinical interventions. Download: Download high-res image (160KB) Download: Download full-size image
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高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2019
·
IF 2.813
Zhuowei Shen,Kaifeng He,Mingcheng Xu,Kui Zeng,Jie Pan,Fengting Ou,Jianbiao Yao,Ruwei Wang,Su Zeng
A sensitive and specific bioanalytical method of liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the quantification of 6-hydroxykynurenic acid (6-HKA) in a small quantity of rat plasma has been developed and comprehensively validated. Tolbutamide (Tol) was used as the internal standard (IS). An aliquot of 50 μL rat plasma sample was deproteinized by 150 μL methanol, and then 100 μL of its supernatant was mixed with 100 μL water after centrifugation . Chromatographic separation was performed on a ZORBAX Eclipse Plus C 18 Rapid Resolution HD column (2.1 mm × 100 mm, 1.8 μm) with a gradient mobile phase consisting of water containing 2 mM ammonium formate and methanol at a flow rate of 0.2 mL/min over a total run time of 5.0 min. The mass spectrometer was operated under multiple reactions monitoring (MRM) mode with the transitions m / z 206.1 → 160.0 for 6-HKA and m/z 269.0 → 170.0 for Tol. The linear range was 2.5–250 ng/mL with the square regression coefficient (r 2 ) of 0.997. The lower limit of quantification (LLOQ) was 2.5 ng/mL (Relative Error, RE +1.6% and RSD 4.8%, n = 5). The intra- and inter-day precision and accuracy was <13.3%. The mean recovery of 6-HKA in rat plasma was between the range of 99.3–103.4%. This method was successfully applied to study the pharmacokinetics of 6-HKA in rats after oral administration at a single dose of 20.0 mg/kg and after tail intravenous injection at a single dose of 2.0 mg/kg. Pharmacokinetic parameters bioavailability, C max, oral , T max, oral , AUC 0–24h, oral , AUC 0–∞, oral , AUC 0–24h, iv and AUC 0–∞, iv were 3.96%, 152.0 ± 85.5 ng/mL, 0.4 ± 0.1 h, 340.0 ± 136.3 ng/mL ∗ h, 369.5 ± 135.0 ng/mL ∗ h, 906.6 ± 324.1 ng/mL*h and 932.9 ± 336.5 ng/mL ∗ h, respectively.
研究领域:
分析化学
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药理学
·
生物医学
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DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2023
·
IF 8.8
Youzhi Su,Jianjiang Lu,Jun Liu,Fang Li,Ning Wang,Hongqin Lei,Xiaofang Shen
A modified QuEChERS purification–liquid chromatography-tandem mass spectrometry method has been developed to determine 51 pesticide residues with newly established maximum residue limits (MRLs) in foodstuffs. Samples were extracted with acetonitrile under citrate-buffered conditions and purified using a modified QuEChERS method employing hydroxylated MWCNTs , SAX, and C 18 . The limits of quantification ranged from 0.2 to 9.8 µg/kg. Recoveries in ten different foodstuffs ranged from 70.2% to 117.9%, with relative standard deviations between 2.3% and 19.9% at three spiking levels. This method was applied to analyze 352 market samples, detecting 14 pesticides in 97 samples. Notably, Afidopyropen, cyantraniliprole, and fluxapyroxad residues in vegetables exhibited a consistent pattern of higher levels in the spring and winter and lower levels in the summer and autumn. Moreover, the risk assessments for acute and chronic dietary exposure to the 14 detected pesticides indicated that the %ADI and %ARfD were well below 100%.
研究领域:
分析化学
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食品安全
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环境科学
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PubMed
高影响因子
BULLETIN OF ENVIRONMENTAL CONTAMINATION AND TOXICOLOGY
·
2023
·Vol. 111
·期 4
·1-9
·
IF 2.7
Zheng Handinghong,Wu Qiong,Wu Xiaomao
This study aimed to investigate the dissipation, residues and dietary assessment of kresoxim-methyl in the application of Rosa Roxburghii and soil field using liquid chromatography-tandem mass spectrometry (LC–MS/MS). The results show that kresoxim-methyl in R. roxburghii samples was extracted by acetonitrile and purified by ethyl enediamine-N-propylsilane (PSA), while kresoxim-methyl in soil samples was extracted by acetonitrile and purified by octadecylsilyl solid phase dispersant (C 18 ). 0.1% formic acid (v/v)-water–methanol solution was used as the mobile phase, LC–MS/MS exhibited a good linearity in the range of 0.001–10 mg L −1 . The recoveries of R. roxburghii and soil matrix were 82.48%–102.55%, and the relative standard deviation ( RSD) were 1.13%–4.21%. The limit of detection ( LOD ) and quantification ( LOQ ) of kresoxim-methyl in R. roxburghii and soil samples was 0.50 and 0.60 µg kg −1 , respectively. The dissipation dynamics of kresoxim-methyl in R. roxburghii and soil followed the first-order kinetics, with the half-life of 4.28 and 4.41 days, respectively. The terminal residual amount of kresoxim-methyl in R. roxburghii and soil samples was 0.003–1.764 and 0.007–2.091 mg kg −1 , respectively. The dietary intake risk assessment indicates that a risk quotient ( RQ ) for kresoxim-methyl based on the national estimated daily intake ( NEDI ) of 0.1995 mg was 0.79%, suggesting that the use of kresoxim-methyl on R. roxburghii at recommended dosage was safe to consumers. This study provides the theoretical basis for guiding the rational use of kresoxim-methyl in the production of R. roxburghii .
研究领域:
植物学
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农业科学
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食品科学
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PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2022
·
IF 3.571
Yudan Wang,Jia’ an Qin,Jing Zhang,Ziyue Jin,Jiaoyang Luo,Meihua Yang
Three different imidacloprid hapten structures were designed to conjugate with proteins (bovine serum albumin, BSA; ovalbumin , OVA; keyhole limpet hemocyanin , KLH) for screening the optimal immunogen and coating antigen. Among these, an unreported antigen (hapten 6-KLH) was selected as the optimal immunogen and coating antigen. In addition, an imidacloprid-specific and high titer monoclonal antibody (IMIB7C3) was obtained by using the above-selected immunogen. A sensitive ic-ELISA (indirect competitive enzyme-linked immunosorbent assay) with a half-maximal inhibitory concentration (IC 50 ) of 1.3 ng mL −1 was established by using the IMIB7C3 antibody (only 1.2 ng per well) to detect the residues of imidacloprid in grains (wheat and maize) and different herbs ( Notoginseng radix et rhizoma, Dioscoreae rhizoma, Lonicerae japonicae flos, Astragali radix , Jujubae fructus ). The detection results of real samples by the developed immunoassay were confirmed by liquid chromatography-tandem mass spectrometry (LC–MS/MS), which proved the accuracy and reliability of the established ic-ELISA. These results indicate that the proposed ic-ELISA method is suitable for rapid and high-throughput detection of imidacloprid residues in agricultural products and medicinal herbs. Furthermore, a quantitative risk assessment was conducted for Lonicerae japonicae flos based on the detection results, which indicates an acceptable risk to human health after the intake of Lonicerae japonicae flos polluted by imidacloprid.
研究领域:
农业化学
·
分析化学
·
免疫学
·
药理学
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DOI
PubMed
高影响因子
Acta Pharmaceutica Sinica B
·
2023
·
IF 14.5
Jiawen Yang,Aixuan Zhou,Minyi Li,Qiaoxian He,Jingwei Zhou,Jacques Crommen,Wentao Wang,Zhengjin Jiang,Qiqin Wang
Due to low immobilized ligand density, limited binding capacity, and severe interference from serum proteins, developing ideal peptide-based biomaterials for precise recognition and in vivo analysis of biopharmaceuticals remains a huge challenge. In this study, mimotope peptide modified pompon mum-like biomimetic magnetic microparticles (MMPs, 3.8 μm) that mimic the specific functionalities of CD20 on malignant B cells were developed for the first time. Benefit from the numerous ligand binding sites (Ni 2+ ) on the pompon mum-like MMPs, these novel materials achieved ≥10 times higher peptide ligand densities (>2300 mg/g) and antibody binding capacities (1380 mg/g) compared to previous reported biomaterials. Leveraging the high specificity of the mimotope peptide, rituximab can be precisely recognized and enriched from cell culture media or serum samples. We also established an LC‒MS/MS method using the MMPs for tracking rituximab biotransformation in patient serum. Intriguingly, deamidation of Asn55 and Asn33, as well as oxidation of Met81 and Met34 were observed at the key complementarity determining regions of rituximab, which could potentially influence antibody function and require careful monitoring. Overall, these versatile biomimetic MMPs demonstrate superior recognition and enrichment capabilities for target antibodies, offering interesting possibilities for biotransformation analysis of biopharmaceuticals in patient serum.
研究领域:
生物技术
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药学
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分析化学
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生物化学
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DOI
PubMed
高影响因子
PROCESS BIOCHEMISTRY
·
2023
·
IF 4.4
Xiaoxuan Cai,Miaoen Huang,Xixiang Huang,Huan Liu,Tianji Wang,Li Li,Weiguang Yang,Hui Luo,Yingnian Lu
The organism Sipunculus nudus L is a good resource for marine peptides because of its rich protein. However, the disadvantage of biological peptides is their short metabolic half-life, therefore, structural modification of peptides is necessary. In this research, the enzymatic hydrolysis of Sipunculus nudus L was performed using trypsin and then peptides were isolated and purified from the hydrolysates, four novel tripeptides were identified by LC-MS-MS as Ser-Arg-Pro (SRP, m/z = 358.39), Pro-Arg-Pro (PRP, m/z = 368.43), Arg-Pro-Ala (RPA, m/z = 342.39), and Lue-Pro-Lys (LPK, m/z = 356.46), their ACE inhibitory activity was investigated with IC 50 value as following 0.046, 0.42, 0.97, and 6.54 mM, respectively. Because of its highest ACE inhibitory activity, SRP was further selected to modify the chemical structure for a sustained release agent DSPE-PEG-SRP. Compared with 7 h of free SRP, the release of DSPE-PEG-SRP in vitro was approximately 120 h. The ACE inhibition rate of SRP released from the synthetic product and the raw material SRP was almost the same, molecular docking demonstrated that ACE inhibitory activity was attributed to the formation of hydrogen bonds between SRP and ACE active sites . In conclusion, DSPE-PEG-SRP, a novel sustained release agent, has great potential and is expected to be further applied to treat hypertension.
研究领域:
海洋生物学
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药学
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生物化学
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高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2025
·
IF 2.8
Bohan Liang,Yanjie Li,Lingmei Xu,Li Wang,Quankun Zhuang,Shiqi Dong,Huirong Fan
XZP-3287(bireociclib) is a novel and selective inhibitor of the cell cyclin-dependent kinases 4/6 (CDK4/6), which is primarily employed for the treatment of breast cancer in clinical trials . In this study, a novel and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the simultaneous determination of XZP-3287 and its metabolites XZP-5286, XZP-3584 and XZP-5736 in human plasma in accordance with international conference on harmonization of technical requirements for registration of Pharmaceuticals for Human use (ICH) guideline R3 (M10) guideline. The multiple reaction monitoring mode (MRM) of mass spectrometer was used and all compounds were monitored in electrospray ionization (ESI+) mode. The correlation coefficients (R 2 ) of all calibration curves for linear regression were greater than 0.99. The intra- and inter-day precision of XZP-3287 and its metabolites XZP-5286, XZP-3584 and XZP-5736 were determined to be 5.2 %–5.5 %, 14.9 %–10.1 %, 6.9 %–13.8 % and 7.3 %–5.6 %, and their accuracy were determined to be 5.2 %–6.0 % 6.9 %–4.4 %, 11.1 %–5.0 % and 7.4 %–5.6 %, respectively. In conclusion, a method for the simultaneous detection of the pharmacokinetic profiles of XZP-3287 and its metabolites in human plasma had been successfully developed. The results demonstrated the efficacy, sensitivity, and reliability of this method
研究领域:
药物分析
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临床药理学
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肿瘤学
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质谱分析
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药物代谢
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生物分析化学
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DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）