JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2022
·
IF 3.318
Hua Li,Yang Wang,Ru Ding,Chen Chen,Zhixuan Tian,Hongnan Yin,Lieming Ding
A sensitive and reliable method was developed to determine befotertinib (D-0316) and its metabolite D-0865 from human plasma by LC-MS/MS. The samples were prepared by simple protein precipitation and 2 µL of the supernatant were chromatographed on a C18 analytical column (ACE Excel 2 Super C 18 , 50 × 2.1 mm). Elution was performed with mobile phase A (10 mM ammonium acetate in water containing 1 % formic acid) and mobile phase B (acetonitrile containing 1 % formic acid) under a gradient program in a total run time of 4 min. Triple Quadruple 5500 equipped with Turbo Ion Spray source and multiple reaction monitoring (MRM) were used for the analysis detection. The transitions were m / z 568.3 → 72.1 m / z (befotertinib), m / z 554.2 → 497.2 (D-0865), and m / z 455.2 → 164.9 (verapamil, internal standard). According to the Chinese Pharmacopeia Commission and ICH Harmonised Guideline for Bioanalytical Method Validation, this method was validated within the spectrum of its accuracy, precision, selectivity, linearity, recovery, matrix effect, and stability. This LC-MS/MS method was successfully applied for the quantitation of befotertinib and its metabolite D-0865 in human plasma during the pharmacokinetics study of befotertinib in non-small cell lung cancer (NSCLC) patients.
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高影响因子
Metabolites
·
2022
·Vol. 12
·期 9
·841
·
IF 5.581
Simeng Zhang,Yuchan Deng,Annan Zhang,Lili Yan,Zhichao Zhang,Jing Wei,Qiang Zhang
The transitional expression and aggregation of amyloid β (Aβ) are the most important causative factors leading to the deterioration of Alzheimer’s disease (AD), a commonly occurring metabolic disease among older people. Antioxidant agents such as vitamin C (Vc) have shown potential effects against AD and aging. We applied an liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) method and differential metabolites strategy to explore the metabolic disorders and Vc restoration in a human Aβ transgenic (Punc-54::Aβ1–42) nematode model CL2006. We combined the LC-MS/MS investigation with the KEGG and HMDB databases and the CFM-ID machine-learning model to identify and qualify the metabolites with important physiological roles. The differential metabolites responding to Aβ activation and Vc treatment were filtered out and submitted to enrichment analysis. The enrichment showed that Aβ mainly caused abnormal biosynthesis and metabolism pathways of phenylalanine, tyrosine and tryptophan biosynthesis, as well as arginine and proline metabolism. Vc reversed the abnormally changed metabolites tryptophan, anthranilate, indole and indole-3-acetaldehyde. Vc restoration affected the tryptophan metabolism and the biosynthesis of phenylalanine, tyrosine and tryptophan. Our findings provide supporting evidence for understanding the metabolic abnormalities in neurodegenerative diseases and the repairing effect of drug interventions.Keywords:Alzheimer’s disease;dementia;neurodegenerative disease;aging;Aβ;metabolism;amino acid;ascorbic acid
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JOURNAL OF LIPID RESEARCH
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2021
·Vol. 63
·期 1
·
IF 5.922
Rui Peng,Juan Le,Shu-Lin Yang,Jing-Ru Cheng,Yan Li,Shao-Ting Wang
Sex hormones, including androgens, estrogens, and progestogens, are important biomarkers for various diseases. Quantification of sex hormones is typically conducted by LC-MS/MS. At present, most methods require liquid-liquid extraction or solid phase extraction for sample preparation. However, these pretreatments are prone to compromise LC-MS/MS throughput. To improve on the current standard practices, we investigated cold-induced phase separation for sex hormone extraction. After protein precipitation with acetonitrile and adjusting the solution constitution with water, samples were stored at −30°C for 10 min to generate two distinct phases: an acetonitrile-rich layer on top of a water-rich layer. During this process, the hydrophobic sex hormones spontaneously separate into the upper layer. This simple and reliable cold-induced phase separation-based LC-MS/MS methodology was used here to simultaneously detect estrone, estradiol, estriol, testosterone, androstenedione, dehydroepiandrosterone, progesterone, and 17-hydroxyprogesterone in serum. Validation of this method indicated satisfactory performance, including acceptable linearity, accuracy, precision, and tractability. Compared with the mainstream liquid-liquid extraction-based method, this new method exhibits significant progress in throughput, which shortens the time cost of sample preparation from 90 to 40 min. We propose that this method can be an excellent alternative for sex hormone analysis in routine clinical laboratories.
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FOOD CHEMISTRY
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2021
·
IF 7.514
Renyong Liao,Qiang Xia,Changyu Zhou,Fang Geng,Ying Wang,Yangying Sun,Jun He,Daodong Pan,Jinxuan Cao
The spoiled dry-cured ham commonly shows unpleasant taste and odour. To deepen the understanding in the formation mechanism of unpleasant taste in spoiled ham, sensory attributes, texture parameters, protein degradation, metabolites were investigated between normal and spoiled hams; the relationship between the sensory quality and metabolites of dry-cured ham was further evaluated by partial least square discriminant analysis (PLS-DA). The scores of richness and overall acceptance were significantly lower in spoiled ham, and more than 12.5-fold values in adhesiveness were found in spoiled ham than normal ham. Myofibrillar proteins including actin, troponin-T and myosin light chain showed excessive degradation in spoiled ham. Forty-two kinds of metabolites mainly derived from protein degradation were identified by LC-MS/MS, and amino acid derivatives and oligopeptides were the key components to distinguish spoiled and normal hams demonstrated by PLS-DA. Purine metabolism, pyrimidine metabolism and protein degradation were the main metabolism pathways in spoiled ham.
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ANALYTICAL BIOCHEMISTRY
·
2021
·
IF 3.365
Yan-Ying Xu,Fei Qin,Yi-Xin Dai,Xue-Feng Zhong,Juan Yan,Su-Mei Xu,Ping-Sheng Xu
This study aimed to develop an LC-MS/MS method for determining sildenafil and its metabolites N -desmethylsildenafil and N1,N4 -desmethylsildenafil in human plasma and applying it to a pharmacokinetic study of sildenafil in healthy volunteers. Sildenafil-d8 was used as the internal standard. Plasma samples were pretreated via protein precipitation with acetonitrile . The extractives were then separated on an ACQUITY UPLC BEH C18 (50-mm × 2.1-mm, 1.7-μm) column using gradient elution . The aqueous and organic mobile phases were ammonium formate 2 mM supplemented with 0.1% formic acid in water and acetonitrile, respectively, and the flow rate was 0.3 mL/min. An electrospray ionization source was applied, and multiple reaction monitoring was operated in the positive mode with selective channels at m / z 475.30 → 100.10, 461.20 → 283.30, 483.30 → 108.10, and 449.00 → 283.00 for sildenafil, sildenafil-d8, N - desmethylsildenafil, and N1,N4 -desmethylsildenafil, respectively. The linear calibration curves of sildenafil and its metabolites spanned 1.0–1000 ng/mL. The lower limit of quantification was 1.0 ng/mL. The extractive recovery of analytes from the biological matrix was more than 90% and the matrix effect complied with relevant provisions. The intra- and inter-day precisions of sildenafil and its metabolite were <10%. The intra- and inter-day accuracy of sildenafil, N - desmethylsildenafil, and N1,N4 -desmethylsildenafil was more than 99%. The method is highly sensitive and selective, and it was successfully applied to the bioequivalence studies of 100-mg sildenafil citrate tablets in 40 healthy Chinese volunteers.
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高影响因子
Analytical Methods
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2021
·Vol. 13
·期 29
·3242-3248
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IF 2.896
Pengpeng Zhang,Shuai Liu,Shuang Yang,Yuanhong Wang,Tingfu Jiang,Mingming Yu,Zhihua Lv
A simple and sensitive method for the simultaneous determination of chito-oligosaccharides (COSs) with degrees of polymerization (DPs) from 2 to 7 was developed and used for COS quantification in rat plasma. Samples were separated on a Waters XBridge Amide column (3.5 μm, 2.1 × 150 mm) by isometric elution with 10 mM aqueous ammonium acetate (pH = 9) in acetonitrile and 10 mM aqueous ammonium acetate (pH = 9) (v/v, 50 : 50) employing multiple reaction monitoring (MRM) detection. Analytes and internal standards (IS) were extracted from rat plasma by protein precipitation with acetonitrile. The assay was linear over a concentration range of 20–10 000 ng mL−1 for COS2–7. The intra-day and inter-day precision of the investigated components exhibited an RSD within 15%, and the accuracy (RE%) ranged from −7.3% to 7.6%. The extraction recoveries of the six constituents were determined to be between 82.5% and 94.3%. No significant matrix effects for COS2–7 were observed in rat plasma. COS in plasma remained stable for 24 h at room temperature (short-term), after freeze–thaw cycles, and 30 days in a −40 °C freezer. In comparison to reported COS quantitation methods, this method is simple, sensitive and cost-effective and could be used for the simultaneous quantitation of COS2–7. This method meets the Food and Drug Administration guidelines and had been successfully applied to the analysis of pharmacokinetic samples collected from rats.
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XENOBIOTICA
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2020
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IF 1.902
Luyu Bai,Qingsong Fei,Fang Lei,Rui Luo,Qun Ma,Manman Dai,Huimin Zhang,Ning He
The objective of this study was to compare the pharmacokinetics of vancomycin hydrochloride administered into rabbits through different routes and explore the feasibility of peptide drugs entering the systemic circulation through ocular administration.A convenient, accurate, and rapid liquid chromatography-trandem mass spectrometric (LC-MS/MS) method was established and used for the determination of vancomycin hydrochloride in rabbit plasma after intravenous administration (1.5 mg/kg), intragastric, and ocular administration (15 mg/kg). The pharmacokinetic parameters were analyzed using the DAS 2.0 software.We obtained a linear calibration curves vancomycin hydrochloride in plasma of rabbits over a concentration range of 0.05–10.0 μg/mL (R2 > 0.9995), the interassay accuracy was within 5%, precision of 1.66–3.38%, and recovery of >85%. No matrix effects were observed. The absolute bioavailability of vancomycin hydrochloride after intragastric and ocular administration was 1.0 and 7.3%, with the half-life values of 63.1 and 138.5 min, respectively.Therefore, the LC-MS/MS method established in this experiment was suitable for the determination of vancomycin hydrochloride. Vancomycin hydrochloride was rapidly absorbed into the blood circulation after ocular administration. Ocular administration was linked to higher bioavailability compared with intragastric administration, suggesting that the former will become a route for the delivery of peptide drugs.
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Food Bioscience
·
2024
·
IF 4.8
Qi Sun,Guangqing Mu,Peng Sun,Qing Zhao,Xiaomeng Wu,Fanhua Kong
Casein (CN) is the primary factor leading to allergic reactions in infants to bovine milk, severely limiting the intake of bovine milk formula by allergic infants. This study investigates the conformational changes and regulation of linear epitopes during the hydrolysis of CN by five proteases derived from microbial and plant sources using multiple spectroscopic techniques combined with LC/MS-MS. The results showed that the IgE inhibition rates for SD (subtilisin hydrolysate), PD (papain hydrolysate), BD (bromelain hydrolysate), KD (proteinase K hydrolysate), and FD (ficin hydrolysate) were 43.19%, 41.99%, 35.45%, 48.15%, and 14.80%, respectively. The differences in antigenic residues remaining after hydrolysis by different proteases mainly result from the varying degrees of structural alteration of CN and the hydrolysis allergic epitope regions. This study provides theoretical basis for understanding the mechanism by which proteases reduce the allergenicity of CN. It also offers new insights into the development of multienzyme combinatorial hydrolysis strategies.
研究领域:
食品科学
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免疫学
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生物化学
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高影响因子
JOURNAL OF SEPARATION SCIENCE
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2021
·Vol. 44
·期 20
·3799-3809
·
IF 3.645
Xu-zhao Li,Shuai-nan Zhang,Qi Liu,Wu-de Yang,Ying Zhou
Herba Lysimachiae inhibits synovial damage in osteoarthritis via regulating two bio labels (integrin alpha 2b/beta 3). However, the relevant active ingredients are still unknown. Here, the active ingredients of herbal medicines were analyzed based on the liquid chromatography–tandem mass spectrometry technology and public bioinformatics platforms. The liquid chromatography–tandem mass spectrometry technology was used for compound analysis, and public databases (PubChem BioAssay and STRING) were applied to establish the links between herbal compounds and both bio labels, and identify which herbal compounds may regulate these bio labels. Subsequently, the osteoarthritis model was used to confirm the results. Totally, ninety compounds in Herba Lysimachiae were identified based on the liquid chromatography–tandem mass spectrometry technology. Bioinformatics analysis showed that five compounds (myricetin, fisetin, esculetin, 7-hydroxycoumarin-4-acetic acid, and caffeic acid) may synergistically regulate bio labels through 11 targets, which may be the active ingredients of Herba Lysimachiae for osteoarthritis treatment. In the verification experiments, five compounds markedly suppressed the overexpression of bio labels in the synovium of the osteoarthritis model. In conclusion, the present study effectively and rapidly analyzed the active ingredients of Herba Lysimachiae for osteoarthritis treatment.
研究领域:
药理学
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生物信息学
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分析化学
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风湿病学
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高影响因子
MICROCHEMICAL JOURNAL
·
2026
·
IF 5.2
Liang Li,Wanting Gao,Xinyan Chen,Meijia Liu,Wei Long,Qunyin Zhu
NH₂-MCOF enables ultra-sensitive detection of 17 PFASs down to 0.0346 ng/L. • Fast MSPE within 40 min and reusable for ≥6 cycles with stable performance. • Successfully detected PFASs in real urban waters, including 3.346 μg/L PFDS. Per - and polyfluoroalkyl substances (PFAS), as a class of persistent organic pollutants, are characterized by strong environmental persistence and high bioaccumulation potential, making them a major concern in global environmental and health fields. Currently, the trace detection of PFASs in urban environmental water samples, including surface water, source water, and domestic wastewater faces challenges such as insufficient adsorption selectivity of traditional materials and cumbersome pretreatment steps, highlighting the urgent need to develop efficient enrichment and highly sensitive analytical methods. To improve the enrichment efficiency of PFAS, this study designed and synthesized an amino-functionalized magnetic covalent organic framework material (NH₂-MCOF) as an adsorbent. Combined with magnetic solid-phase extraction (MSPE) and liquid chromatography-tandem mass spectrometry, a synchronous analytical method was established for the determination of 17 PFASs in real urban environmental water matrices. Through systematic optimization, the optimal pretreatment conditions were determined as follows: adsorbent dosage of 20 mg, solution pH of 3.0, ultrasonic-assisted adsorption time of 40 min, and a stepwise elution strategy using methanol, ammoniated methanol, and formic acid-modified methanol. Under the optimized conditions, the method demonstrated good linearity within the range of 0.5–200 μg/L, with detection limits of 0.0346–1.30 ng/L. The spiked recoveries ranged from 50% to 138%, and the intra -day and inter -day precision, expressed as relative standard deviations (RSD), were below 13.5% and 14.9%, respectively. Application to real water samples confirmed the method's effectiveness in detecting multiple PFASs, demonstrating its practicality and reliability. The analytical method established in this study integrates functionalized material design, efficient pretreatment, and sensitive detection, providing a reliable approach for the synchronous monitoring of multiple trace PFAS in real urban environmental water matrices and highlighting the potential application of functionalized magnetic covalent organic framework materials in environmental analysis. Download: Download high-res image (103KB) Download: Download full-size image
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高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2026
·
IF 4.1
Yang Shuang,Wan Wei,Qu Ziyu,Yi Keke,Zhang Di,Jiang You,Ye Zihong,Fang Xiang,Xie Jie,Dai Xinhua
Steroid hormones play crucial regulatory roles in human growth, development, reproduction, and the maintenance of internal environmental homeostasis. Because the concentrations of most hormones in the body are extremely low and their chemical properties vary widely, developing an accurate and sensitive quantitative method has become a primary objective in clinical diagnostics. In this study, an isotope dilution liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS) method was developed and validated for the simultaneous quantification of 22 steroid hormones in human serum. To enhance extraction and purification efficiency, a protein precipitation–solid-phase extraction (PP-SPE) approach was employed, forming a “dual purification” strategy. The limits of quantification for progesterone, cortisol, dihydrotestosterone, and dehydroepiandrosterone sulfate were 0.05, 0.50, 0.05, and 1.00 ng/mL, respectively, representing an improvement over previously reported values obtained using similar sample pretreatment methods. Method validation results demonstrated strong linearity for all 22 steroid hormones ( R 2 > 0.98). Accuracy ranged from 86.9% to 119.5%, intra-day precision was below 9.7%, inter-day precision was below 12.0%, and the matrix effect was controlled within 80.3%–118.1%. These findings indicate that the method is accurate, reliable, and suitable for analyzing multiple components in complex serum matrices. Twenty real serum samples were analyzed to evaluate the clinical applicability of the method. The results demonstrated that this method can be used clinically to monitor steroid hormone levels, assist in diagnosing and treating endocrine disorders, and provide a diagnostic basis for adrenal diseases. It holds significant reference value for clinical laboratory testing. Graphical
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高影响因子
Talanta Open
·
2025
·
IF 3.7
Bao Sun,Zhaodi Xia,Chen Wang,Ru Tie,Mengyao Wu,Yilin Ru,Yaxi Meng,Lu Bai,Ying Zhang,Pu Jia,Shixiang Wang,Bing Qi,Xiaohui Zheng
Sensitive and comprehensive measurement of systemic metabolites of Trp, Phe and Glu in biological samples is effective for understanding the pathogenesis of pain, anxiety, depression, PTSD and other neurological diseases. This study developed a LC-MS/MS method for simultaneous monitoring the 10 neurotransmitters in mouse hippocampus, and applied it to investigate their changes in five neuroinflammatory mouse models. The quantitative analysis of 10 neurotransmitters, including Gamma-aminobutyric acid (γ-GABA), L-Glutamate (Glu), L-Glutamine (Gln), L-Tryptophan (Trp), Serotonin (5-HT), 5-Hydroxyindoleacetic acid (5-HIAA), L-Phenylalanine (Phe), L-Tyrosine (L-Tyr), Dopamine (DA), Levodopa (L-DOPA) was achieved within a chromatographic separation time of 4.5 min by the application of ThermoFisher Scientific™ Vanquish™ HPLC coupled to ThermoFisher ScientificTM TSQ QuantisTM mass spectrometer. Optimized chromatographic separation as well as high sensitivity allow the simultaneous analysis and precise quantification of ten neurotransmitters in mouse hippocampus. The limits of detection in sample ranged from 0.3pg (Phe) to 0.1 μg (γ-GABA). Recoveries were between 88.0 to 113.8 %, the mean intra - day and inter - day coefficient of variation of 5.56% and 4.72%, respectively. The matrix effect was from 85.1 to 114.9%. A series of significant changes in five neuroinflammatory mouse models can be detected. γ-GABA, Glu, Gln, DA, Phe, L-Tyr, 5-HIAA were decreased in depression model. Gln and Glu were decreased in PTSD model. 5-HIAA was elevated in anxiety. 5-HIAA and L-Trp were decreased in CFA and SNI model, respectively. In conclusion, a LC-MS/MS method for simultaneous measurement of 10 neurotransmitters in mouse hippocampus was developed and successfully applied to investigation of the changes in five neuroinflammatory mouse models. The method would be expected to provide applicability to the study of the mechanisms of neurological diseases associated with these neurotransmitters.
研究领域:
神经科学
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分析化学
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药理学
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