JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2021
·
IF 3.935
Mei Qu,Peng Xue,Qi Zhang,Tiantian Lu,Kun Liu,Bingying Hu,Jingjing Pang,Qianqian Xiao,Tongxin Xu,Quande Wang,Zhongzhe Cheng
Solasodine , a major ingredient in Solanaceae family, has various biological functions such as inducing neurogenesis, anticonvulsant and anti-tumor. Its risk assessment has also drawn public attention. However, little is known about its oral bioavailability and metabolic process. In this study, an liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the quantification of solasodine in mice dried blood spot (DBS) samples. To block nonspecific adsorption, DBS samples were pretreated with bovine serum albumin (BSA) and then extracted with ethyl acetate . This method was applied to a pharmacokinetic and bioavailability study of solasodine. The absolute bioavailability was only 1.28%. Thereafter, its metabolites in mice were characterized using an ultra-performance liquid chromatography Q-Exactive high-resolution mass spectrometer (UHPLC-QE-HRMS). Several isomeric metabolites were well separated and differentiated using their retention time, fragmentation pathways and correspondingly fragmentation rules of solasodine. As a result, 21 metabolites were characterized including 16 phase I and 5 phase II metabolites. The proposed metabolic pathways showed that solasodine mainly experienced oxidation, dehydration, dehydrogenation and sulfation. These results could help us to better understand the efficacy and safety of solasodine.
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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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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ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2021
·Vol. 414
·期 4
·1553-1561
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IF 4.157
Zhang Wenjuan,Hu Haoyun,Ruan Guihua,Huang Yipeng,Du Fuyou,Chen Zhengyi
In this study, reduced graphene oxide (rGO) hybridized high internal phase emulsions were developed and polymerized as porous carriers for aptamer (5’/5AmMC6/-AGT CCG TGG TAG GGC AGG TTG GGG TGA CT-3’) modification to enrich human α-thrombin from serum. The structure and properties of the materials were confirmed by scanning electron microscope (SEM), Fourier transform infrared spectroscope (FT-IR), and X-ray photoelectron spectra (XPS). The adsorption ability and selectivity were studied and the thrombin was detected with liquid chromatography-mass spectrometry (LC–MS). The adsorption of thrombin onto the sorbent was achieved within 30 min and the desorption was realized using 5.0 mL of acetonitrile/water (80/20, v/v). The thrombin was quantified by LC–MS according to its characteristic peptide sequence of ELLESYIDGR. Graphical abstract
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TALANTA
·
2020
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IF 5.339
Weiwei Ma,Shuangfeng Wan,Chenchen Lin,Xucong Lin,Zenghong Xie
Highly specific sample pretreatment for the sensitive detection of trace bisphenol A (BPA) in compliacted samples is critical. Herein, a new protocol towards online specific recognition and sensitive detection of BPA was proposed by using [email protected] affinity monolith coupled with LC-MS. Optimization of polymerization conditions and characterization such as the morphology, energy spectrum, mechanical stability, aptamer coverage density and specific performance of the affinity monolith were studied. Nano-gold particles (AuNPs) densely distributed on the rigid hybrid-silica substrates, and an unusually high aptamer coverage density reached 3388 pmol/μL, which was favorable to fulfill the effective identification of BPA with high selectivity and inhibit the interference of analogs including BPB and BPC. A highly sensitive recognition of BPA was obtained with the limit of detection (LOD) as low as 0.02 ng/mL. Applied to dairy milk products and serum samples, trace BPA could be sensitive detected by this strategy, while the poor response was achieved by using traditional non-specific SPE column for sample pretreatment. Satisfactory recoveries of fortified BPA were measured as 97.45 ± 2.24%–98.03 ± 4.36% (n = 3) in powdered infant formulas, 96.64 ± 3.37% ~ 99.42 ± 3.22% (n = 3) in bottled milk, 94.69 ± 2.15% ~ 100.96 ± 1.94% (n = 3) in boxed milk, and 93.71 ± 1.53% ~ 96.73 ± 2.56% (n = 3) in children serum samples, respectively. This protocol lights a new access to online specific identification of trace BPA from complex matrix with good detection sensitivity by using aptamer-affinity monolithic column.
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XENOBIOTICA
·
2021
·
IF 1.908
Yun-Jing Zhang,Wen-Li Zhou,Fei Yu,Qian Wang,Can Peng,Jia-Yi Kan
Bovis Calculus Artifactus (BCA) is the main substitute for natural Calculus bovis, a traditional drug in China used to treat high fever, convulsion, and sore throat. The effect of BCA on cytochrome P450 (CYP) activities is unknown. This study was to investigate the effect of BCA on eight rat hepatic microsomal CYPisozymes to evaluate the potential drug interactions using the cocktail approach.Metabolites of the eight isoform probe substrates of CYP isozymes were quantified by LC-MS/MS. The method was validated by incubating known CYP inhibitors α-naphthoflavone (CYP1A2), thiotepa (CYP2B1), quercetin (CYP2C7), sulfaphenazole (CYP2C6), ticlopidine (CYP2C11), quinidine (CYP2D1), ketoconazole (CYP3A1),4-methylpyrazole (CYP2E1) with individual probe substrate and rat liver microsomes. The formation rates of the corresponding metabolites of the eight probe substrates were determined to evaluate the activity of each isozyme.The results showed that BCA has different degrees of inhibitory effect on four CYP450 isoforms (CYP2C6, CYP2C11, CYP2D1, CYP3A1) (p < 0.05), but no significant influence on CYP1A2, 2B1, 2C7 or 2E1 (p > 0.05). Attention should be paid to the BCA-drug interactions by careful monitoring and appropriate dosage adjustments in the concurrent use of the drugs which are metabolized by CYP1A2, CYP2C19, and CYP3A4. Abbreviations: BCA, bovis calculus artifactus; CYP, cytochrome P450; DDIs, drug-drug interactions; ESI, electrospray ionization; MRM, multiple reaction monitoring; NBC, Natural Bovis Calculus; QC, quality control; T CM, traditional Chinese medicine.
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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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.
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JOURNAL OF SEPARATION SCIENCE
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2019
·Vol. 42
·期 20
·3234-3242
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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.
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CHIRALITY
·
2018
·Vol. 30
·期 12
·1277-1286
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IF 1.833
Lu-Ning Sun,Yi-Wen Shen,Yu-Wen Ying,Duo Li,Teng-Fei Li,Xue-Hui Zhang,Ping Zhao,Li Ding,Yong-Qing Wang
Rabeprazole is an effective proton pump inhibitor to treat acid-related diseases. To achieve the simultaneous determination of rabeprazole enantiomers in human plasma, a chiral LC-MS/MS method was developed and validated. Acetonitrile including 0.1% ammonium were used as protein precipitating agent. Analytes were separated within 8 minutes on a Chiralpak IC column (4.6 mm × 150 mm, 5 μm). The mobile phase was 10 mM ammonium acetate including 0.2% acetic acid-acetonitrile (35:65, v/v). An API 4000 mass spectrometer was used as detector for the analysis, and the multiple reactions monitoring transitions of m/z 360.1 → 242.2 and 346.1 → 198.1 were opted for quantifying rabeprazole enantiomers and internal standard. Matrix effects were not apparent for each enantiomer and internal standard (esomeprazole), the calibration curves were linear over the concentration of 0.500 to 400 ng·mL −1 , the intra-run precisions were below 5.4%, the inter-run precisions were below 9.9%, and the accuracy was between −9.2% and 9.3%. There was no chiral inversion observed during sample storage, preparation procedure, and analysis, demonstrating that analytes were stable in this study. This method was applied to the stereoselective pharmacokinetic study of (R)-(+)- and (S)-(−)-rabeprazole after oral administration of 10-mg rabeprazole sodium enteric-coated tablet in healthy Chinese subjects.
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CHROMATOGRAPHIA
·
2018
·Vol. 81
·期 12
·1673-1684
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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
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2015
·Vol. 407
·期 24
·7359-7368
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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
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MICROCHEMICAL JOURNAL
·
2024
·
IF 4.9
Fuyang Gu,Ziting Ma,Yannuo Liu,Xiaoyan Wang,Peng Du,Yang Jiang,Guowei Xiao,Yanmei Qu,Changhai Xu
The blend of hydrogen peroxide (H 2 O 2 ) and N-[4-(triethylaminomethyl)benzoyl]caprolactam chloride (TBCC) boosts exceptional bleaching efficacy under low temperature and weak alkaline conditions, greatly reducing energy consumption. Nevertheless, the intricate perhydrolysis pathway of TBCC within a hydrogen peroxide solution and its subsequent impact on the whiteness of fabrics during this process have remained elusive. This study presents an integrated analytical methodology that harnesses ultraviolet spectrophotometry, fluorescent probes, confocal fluorescence microscopy, and liquid chromatography-mass spectrometry (LC-MS) to examine the pivotal aspects of the cotton fabric bleaching process. Specifically, we focus on the detection and quantification of the critical product N-4-(triethylammoniomethyl)peracetic acid (TPA) in the bleaching reaction. The research detected and quantified TPA, while emphasizing that insufficient concentrations and abbreviated durations of TPA significantly compromise the bleaching efficacy. Notably, variations in the TPA generation rate under different conditions revealed why TBCC exhibits exceptional bleaching performance under low-temperature and mildly alkaline conditions. This insight provides new perspectives and valuable insights into the critical factors influencing the bleaching process. The method is also applicable to other bleaching activators, and by controlling these factors in conjunction with actual conditions, it is possible to effectively reduce energy waste and provide valuable information for optimizing future practices in the field of bleaching.
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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.
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危险品化学品经营许可证（带存储）