SPECTROCHIMICA ACTA PART A-MOLECULAR AND BIOMOLECULAR SPECTROSCOPY
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2024
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IF 4.3
Zhu-Rui Zhang,Ying Chen,Zhi-Wei Wang,Chang-Ying Hu,Yuling Hu,Xiaowen Xu
Polylactic acid (PLA) straws hold eco-friendly potential; however, residual diisocyanates used to enhance the mechanical strength can generate carcinogenic primary aromatic amines (PAAs), posing health risks. Herein, we present a rapid, comprehensive strategy to detecting PAAs in 18 brands of food-grade PLA straws and assessing their migration into diverse food simulants. Surface-enhanced Raman spectroscopy was conducted to rapidly screen straws for PAAs. Subsequently, qualitative determination of migrating PAAs into various food simulants (4 % acetic acid, 10 % ethanol, 50 % ethanol) occurred at 70 °C for 2 h using liquid chromatography-mass spectrometry. Three PAAs including 4,4′-methylenedianiline, 2,4′-methylenedianiline, and 2,4-diaminotoluene were detected in all straws. Specifically, 2,4-diaminotoluene in 50 % ethanol exceeded specific migration limit of 2 μg/kg, raising safety concerns. Notably, PAAs migration to 10 % and 50 % ethanol surpassed that to 4 % acetic acid within a short 2-hour period. Moreover, PLA straws underwent varying degrees of shape changes before and after migration. Straws with poly(butylene succinate) resisted deformation compared to those without, indicating enhanced heat resistance, while poly(butyleneadipate-co-terephthalate) improved hydrolysis resistance. Importantly, swelling study unveiled swelling effect wasn’t the primary factor contributing to the increased PAAs migration in ethanol food simulant, as there was no significant disparity in swelling degrees across different food simulants. FT-IR and DSC analysis revealed higher PAAs content in 50 % ethanol were due to highly concentrated polar ethanol disrupting hydrogen bonds and van der Waal forces holding PLA molecules together. Overall, minimizing contact between PLA straws and alcoholic foods is crucial to avoid potential safety risks posed by PAAs.
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JOURNAL OF PHARMACOLOGICAL AND TOXICOLOGICAL METHODS
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2024
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IF 1.3
Lingjiao Wang,Mengqiang Zhao,Jiao Li,Hongtao Xu,Yang Song,Yuanyuan Zhao,Jing Yu,Chunhua Zhou
Background Therapeutic drug monitoring for antidepressants (ADs) is vital due to the potentially serious consequences and disputes related to medical events. Therefore, we created a quick and convenient analysis way for separation and quantification of ADs. Methods To ensure quantitative stability, we divided the 16 ADs or their metabolites into 4 pools (AD1-AD4), considering the hospital frequency that the clinician prescribed, the physicochemical properties of medicines, and the calibration range of selected ADs. After precipitation with methanol, the analytes were eluted for at least 3.5 min on a BEH C 18 analytical column by different gradient elution methods. Results: The LLOQ and LOD were 1.25–10 ng/mL and 0.42–5 ng/mL, respectively. High precision (<12 %) and accuracy (87.07–111.47 %) were demonstrated by quality control samples both within and between days. All the compounds were stable at room temperature and within −80 °C. Conclusion The method is of wide clinical and laboratory interest due to simpler sample cleanup, shorter chromatographic run times, and wider calibration range compared to other methods.
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2024
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IF 2.8
Wenchan Deng,Chundan Ye,Wei Wang,Rongrong Huang,Cheng Guo,Yuanjiang Pan,Cuirong Sun
Colorectal cancer (CRC) is a common malignant tumor in the gastrointestinal tract. Changes in amino acid metabolites have been implicated in tumorigenesis and disease progression. Biomarkers on the basis of chiral amino acids, especially D-amino acids, have not been established for early diagnosis of CRC. Quantification of chiral amino acids, especially very low concentrations of endogenous D-amino acids, is technically challenging. We report here the quantification of L- and D-amino acids in urine samples collected from 115 CRC patients and 155 healthy volunteers, using an improved method. The method of chiral labeling, liquid chromatography, and tandem mass spectrometry enabled separation and detection of 28 amino acids (14 L-amino acids, 13 D-amino acids and Gly). Orthogonal partial least squares discriminant analysis identified 14 targeted variables among these chiral amino acids that distinguished the CRC from the healthy controls. Binary logistic regression analysis revealed that D-α-aminobutyric acid (D-AABA), L-alanine (L-Ala), D-alanine (D-Ala), D-glutamine (D-Gln) and D-serine (D-Ser) could be potential biomarkers for CRC. A receiver operating characteristic curve analysis of combined multi-variables contributed to an area under the curve (AUC) of 0.995 with 98.3 % sensitivity and 96.8 % specificity. A model constructed with D-AABA, D-Ala, D-Gln, and D-Ser achieved an AUC of 0.988, indicating important contributions of D-amino acids to the association with CRC. Further analysis also demonstrated that the metabolic aberration was associated with age and the development of CRC, D-methionine (D-Met) was decreased in CRC patients with age over 50, and D/L-Gln in patients at stage IV was higher than patients at stage I. This study provides the signature of D-amino acids in urine samples and offers a promising strategy for developing non-invasive diagnosis of CRC.
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JOURNAL OF PHOTOCHEMISTRY AND PHOTOBIOLOGY B-BIOLOGY
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2024
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IF 3.9
Lei Ye,Xin Li,Lingzi Zhang,Yu Huang,Bo Zhang,Xuezhen Yang,Wei Tan,Xiaolin Li,Xiaoping Zhang
Light exposure significantly impacted the coloration and metabolism of Auricularia cornea , although the underlying mechanisms remain unclear. This study aimed to test the apparent color and pigment metabolic profiles of A. cornea in response to red (λp = 630 nm) and blue (λp = 463 nm) visible light exposure. Colorimeter analysis showed that fruiting bodies appeared bright-white under red-light and deeper-red under blue-light, both with a yellow tinge. On the 40th day of light-exposure, bodies were collected for metabolite detection. A total of 481 metabolites were targeted analysis, resulting in 18 carotenoids and 11 anthocyanins. Under red and blue light exposure, the total carotenoids levels were 1.1652 μg/g and 1.1576 μg/g, the total anthocyanins levels were 0.0799 μg/g and 0.1286 μg/g, respectively. Four differential metabolites and three putative gene linked to the visual coloration of A. cornea were identified. This pioneering study provides new insights into the role of light in regulating A. cornea pigmentation and metabolic profile.
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CLINICA CHIMICA ACTA
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2024
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IF 3.2
Chen Bu,Liansheng Jiang,Lili Cui,Mao Tang,Xinhua Song,Yingkui Zhao,Zhengyan Liang,Liya Ye,Jiayao Nian,Shouhong Gao,Xia Tao,Zhipeng Wang,Wansheng Chen
Objective To develop a simple, rapid, and sensitive LC-MS/MS method for quantifying 23 tyrosine kinase inhibitors (TKIs) in plasma samples, and evaluate the relationship between the trough concentration of anlotinib(ANL) and its toxicities. Methods The method was developed in Agilent 1290–6460 UHPLC-MS/MS system. This study prospectively enrolled 55 cancer patients undergoing ANL treatment. Plasma samples were collected at steady-state trough concentration and subsequently analyzed using the method. Patients were recorded for the occurrence of toxicities. Statistical analysis was performed to assess the association of the toxicities with ANL exposure level and patients’ characteristics. Results The LC-MS/MS method was developed and validated for all items required by pharmacopoeia. The results revealed a positive association between the trough concentration of ANL and the incidence of toxicities. The exposure level 17.655 ng/mL (AUC 0.82, p = 0.010) was identified as a predictive threshold value for grade ≥ 3 overall toxicities. In addition, lower platelet count (PLT count < 179 × 10 9 g/L) was significantly associated with higher occurrence of grade ≥ 3 toxicities (AUC 0.75, p = 0.049). A logistic model incorporating these two factors demonstrated improved diagnostic capacity for predicting ≥ 3 overall toxicities (AUC = 0.90, p = 0.001). Conclusion This study successfully developed and validated a simple, rapid, and sensitive LC-MS/MS method for quantifying 23 TKIs in plasma samples. Besides, this study found that both C trough of ANL and PLT count as independent predictors for ANL-induced ≥ 3 overall toxicities. Moreover, a logistic model including these two factors presents better prediction capacity for ≥ 3 overall toxicities.
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Analytical Methods
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2024
·Vol. 16
·期 23
·3720-3731
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IF 2.7
Rongrong Cao,Songlin Xu,Zhirui Yu,Liang Xu,Zhiqiang Ge,Qianyu Huo,Guoqing Zhu,Bin Qiao
In recent years, there has been a growing interest in the thriving monoclonal antibody (mAb) industry due to the wide utilization of mAbs in clinical therapies. Robust and accurate bioanalytical methods are required to enable fast quantification of mAbs in biological matrices, especially in the context of pharmacokinetics (PKs)/pharmacodynamics (PDs) and therapeutic drug monitoring (TDM) studies. In this investigation, we presented a novel immuno-magnetic capture coupled with a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method designed for the quantification of immunoglobulin G-kappa-based mAbs in biological fluids. The immunoaffinity absorbent for mAb drug purification was meticulously crafted by immobilizing protein L onto monosize, magnetic poly(glycidyl methacrylate) (m-pGMA) beads, synthesized through dispersion polymerization. The microspheres were acquired with an average size of 1.6 μm, and the optimal binding of mAbs from the aqueous mAb solution was determined to be 45.82 mg g−1. The quantification of mAbs in 10 μL serum samples was achieved through affinity purification using m-pGMA@protein L beads (employing rituximab as an internal standard (IS)), on-bead reduction, and rapid tryptic digestion. Remarkably, the entire process, taking less than 2.5 hours, held significant potential for simplifying pretreatment procedures and minimizing analytical time. Furthermore, the developed method underwent validation in accordance with the European Medicines Agency (EMA) guidelines. The assay demonstrated commendable linearity within the 2–400 μg mL−1 range for both daratumumab and pembrolizumab. Intra- and inter-assay coefficients of variation fell within the range of 0.7% to 13.4%, meeting established acceptance criteria. Other validation parameters also conformed to regulatory standards. Ultimately, the efficacy of the method was substantiated in a pharmacokinetic study following a single-dose intravenous administration to mice, underscoring its applicability and reliability in real-world scenarios.
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY
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2024
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IF 3.8
Yan Qiaofang,Huang Fei,Wang Chuyang,Zhan Min,Zhang Qiaoxuan,Huang Di,Yan Jun,Lin Haibiao,Huang Xianzhang,Han Liqiao
Digoxin, a cardiac glycoside, is widely used in the treatment of cardiovascular diseases. Due to its narrow therapeutic range, precise monitoring of its blood concentration is essential. A reference measurement procedure (RMP) is pivotal for ensuring result accuracy and comparability. The RMP for serum digoxin by ID-LC-MS/MS was optimized with sample pre-treatment and detection processes, and the bracketing calibration method was used, which facilitates more accurate measurement, especially for extreme concentrations. The performance of this optimized RMP was thoroughly evaluated. The limit of detection (LoD) was 0.05 ng/mL (0.06 nmol/L) and the lowest limit of quantification (LLoQ) was 0.10 ng/mL (0.13 nmol/L). The intra- and inter-assay imprecisions were 2.24%, 2.51%, 1.40% and 1.72%, 1.65%, 0.97% at 0.5, 2.0, 5.0 ng/mL, respectively. Recoveries were 99.63 to 101.42% and the linear response ranged from 0.1 to 10.0 ng/mL. The relative bias was 0.41% and 2.00% of our results compared with the median of all participating reference laboratories for IFCC-RELA (External Quality Assessment Scheme for Reference Laboratories in Laboratory Medicine) 2023A and 2023B. The uncertainty, calibration and measurement capability (CMC) of this method were also evaluated. The optimized RMP was applied in the Trueness Verification Plan of Southern China, which indicates significant differences among clinical systems, highlighting the need for standardization efforts. In addition, two commonly used clinical systems which employed immunoassay methods were compared with this optimized RMP, and 26 individual serum samples were analyzed. The good correlations indicate the feasibility of standardization for serum digoxin. The optimized RMP serves as an accurate reference baseline for routine methods, aiming to enhance the accuracy and precision of measurements in clinical laboratories. Graphical Abstract
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MOLECULES
·
2024
·Vol. 29
·期 12
·2856
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IF 4.2
Qin Huang,Hua Zhou,Xianglun Wu,Jiaqi Jiang,Bingdong Zhan,Pinggu Wu
A promising method was established for the determination of nine halobenzoquinones (HBQs) in potable water by membrane solid-phase extraction (MSPE) pretreatment and the liquid chromatography–mass spectrometry (LC-MS) method. A 500 mL water sample was taken for enrichment by the SDB-RPS membrane, which was previously activated by methanol and ultrapure water. The sample was eluted with methanol and re-dissolved with the initial mobile phase after nitrogen blowing. Then, it was detected in negative ion mode using the working curve, and HBQs were quantified by the external standard method. The linearity was satisfactory in the concentration range of 4-1000 ng/L, with correlation coefficients of 0.9963~0.9994. The recoveries were 73.5~126.6% at three spiked levels, with relative standard deviations (RSDs) of 6.8~15.5%. The limits of detection (LOD, S/N = 3) values were 0.1~0.7 ng/L. The results demonstrate that the MSPE-LC-MS method is reliable, rapid, and sensitive for the simultaneous analysis of nine HBPs in potable water.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2024
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IF 3.1
Xina Yu,Shanshan Song,Zhanhua Li,Tiantian Wang,Hui Huang,Qing Shen,Zongyuan Wu,Pei Luo
Panaxynol is a bioactive polyacetylene in food plants; however, its specific benefits in diabetes and metabolic disorders remain unclear. Previous studies have mainly focused on biochemical indicators and clinical evaluations. Limited research has systematically elucidated the beneficial effects of panaxynol from the oxylipins perspective. In this study, we employed an oxylipin analysis platform we previously established using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) based on the multiple reaction monitoring (MRM) method for the profiling of oxylipins. After a 7-week administration of panaxynol to db/db mice, significant alterations in serum oxylipins and potential benefits to hyperglycemia, insulin resistance, and hepatic steatosis were observed. Our analysis also revealed correlations among epoxygenase products derived from arachidonic acid (AA), linoleic acid (LA), and α-linolenic acid (ALA) via cytochrome P450 (CYP) pathways. Furthermore, six potential oxylipins were identified, as offering insights into the mechanisms by which panaxynol may modulate diabetes. These results provide the first in vivo evidence of the impact of panaxynol on oxylipin metabolism and lay the foundation for developing panaxynol as a nutraceutical for diabetes management.
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FOOD CHEMISTRY
·
2025
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IF 9.8
Guijiao Zhao,Ying Zhao,Qianqian Wang,Chenhuan Wang,Chun Wang,Zhi Wang,Qiuhua Wu
Endocrine disrupting compounds (EDCs) in food pose severe threats to human wellness, so it is extremely urgent to develop effective method with high sensitivity for detecting EDCs in seafoods. Herein, novel urea-functionalized magnetic porous polymer (M-NB-POP) was synthesized from N,N,N′,N′-tetra( p -aminophenyl)- p -phenylenediamine and 1,3-bis(2-isocyanato-2-propyl)benzene under mild conditions for the first time. M-NB-POP with good recoverability and recyclability shows excellent adsorption for several typical EDCs through hydrogen bonding, π-π and hydrophobic interaction. Using M-NB-POP as magnetic solid-phase extraction adsorbent, an attractive method for effective enrichment of trace EDCs in red shrimp, river prawn and crayfish was successfully developed prior to LC-MS analysis. The proposed method gave a low detection limit of 1.50–7.80 ng g −1 , high spiked recoveries of 86.3–111 %, and small relative standard deviation of 1.6–6.0 %. This work provides a new protocol for assessment of trace EDCs in seafoods and concurrently presents a new strategy for developing functional materials to enrich organic pollutants.
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FOOD CHEMISTRY
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2025
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IF 9.8
Meng Li,Yanli Dong,Qianqian Wang,Zhi Li,Qiuhua Wu
Herein, two porous organic polymers, triazine functionalized POP (H-CC-POP) as well as triazine and hydroxyl bifunctionalized POP (OH-CC-POP), were prepared for the first time. They were utilized as sorbents for solid-phase extraction (SPE) of neonicotinoid insecticides (NIs). Compared to H-CC-POP, the OH-CC-POP delivered excellent adsorption capacity for NIs through hydrogen bonding and π-π conjugation interactions. A OH-CC-POP based SPE in conjunction with liquid chromatography-mass spectrometry was employed to detect NIs in honey samples. Under optimal conditions, the established OH-CC-POP based method provides a good linear range of 0.70–120 ng g −1 , with coefficients of determination ranging from 0.9940 to 0.9990. A low limit of detection of NIs in honey samples is obtained to be 0.20–0.80 ng g −1 . The method recoveries, measured at three spiking levels, are 82.3–118 %, with a relative standard deviation of lower than 9.7 %. The developed method shows good application prospects for the detection of NIs in complex matrices.
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DRUG RESISTANCE UPDATES
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2024
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IF 15.8
Dajun Gao,Yanting Shen,Lingfan Xu,Yi Sun,Hailiang Hu,Bin Xu,Zhong Wang,Huan Xu
Aims Tumor fatty acid (FA) metabolic plasticity plays a pivotal role in resistance to therapy and poses limitations to anticancer strategies. In this study, our aim is to uncover the role of acetate metabolism in neurodifferentiation (NED)-mediated castration-resistant prostate cancer (CRPC). Methods We conducted analyses using LC-MS/MS on clinical prostate cancer tissue before and after hormone therapy. We established tumor xenograft mouse models, primary tumor cells, and human-derived organoids to detect the novel mechanism of NED and to identify potential therapies. Results The hormone therapy-induced upregulation of acetate metabolism was mediated by acyl-CoA synthetase short-chain family member 2 (ACSS2), which increased c-MYC expression for NED induction. Notably, combined treatment with an ACSS2 inhibitor and enzalutamide significantly reduced the xenograft tumor volume. Conclusion Our findings uncovered the critical role of acetate metabolism in NED-mediated CRPC and suggest that ACSS2 inhibitors may represent a novel, low-toxicity strategy when combined with hormone therapy for treating patients with NED-mediated CRPC.
研究领域:
肿瘤学
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分子生物学
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癌症代谢
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前列腺癌
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激素治疗
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