JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2016
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IF 3.169
Yidi Yang,Xi Zhu,Fei Zhang,Wei Li,Ying Wu,Li Ding
Stress testing was carried out under acidic, alkaline, oxidative, thermal and photolytic conditions to evaluate the intrinsic stability of posaconazole injection. A total of four degradation products were detected and the drug was found to be susceptible to oxidative and thermal degradations. Three unknown degradants formed under oxidative stress condition were isolated by preparative HPLC and unambiguously elucidated by LC–TOF/MS, LC–MS/MS, 1 H NMR, 13 C NMR and 2D NMR techniques. Based on the spectrometric and spectroscopic information, these novel degradation products were unequivocally assigned as the N-oxides of posaconazole. Probable mechanisms for the formation of the degradants were proposed. A new and selective HPLC method was developed and validated to separate, detect and quantify all the degradants in posaconazole injection.
研究领域:
药物分析
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药学
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质谱分析
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核磁共振
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高影响因子
EUROPEAN JOURNAL OF MASS SPECTROMETRY
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2019
·
IF 0.851
Shencong Lv,Henghui Wang,Yong Yan,Miaohua Ge,Jian Guan
A simple, rapid, and efficient liquid chromatography tandem mass spectrometry (LC–MS/MS) method, operated in electrospray ionization and quadrupole linear ion trap modes, has been developed for the identification and structural characterization of aflatoxins in peanuts and its derivative products or bean sauce. Samples (5 g) were extracted with acetonitrile/water/formic acid (79:20:1, v/v). After centrifugation and dilution, the extracts were separated on a C18 analytical column by gradient elution (acetonitrile/0.2% formic acid) and analyzed by UPLC–MS/MS. External calibration was used for qualification. The developed multiple reaction monitoring–information-dependent acquisition–enhanced product ion method enabled quantification and confirmation of the analytes in a single run. Enhanced product ion mode was used for qualitative analysis, while multiple reaction monitoring mode was used for quantitative analysis. An in-house library was constructed for identification. Calibration curves showed good linearity with correlation coefficients (r) higher than 0.994. Limits of detection were determined to be below 0.26 µg kg−1 for most analytes. The recoveries for those substances were in the acceptable range of 80.2%–119.1%. A new LC–MS3 method was established for further confirmation. One pickled pepper peanut was found to contain aflatoxins B1, B2, and G1 with contents of 90.93, 26.64, and 1.92 µg kg−1, respectively.
研究领域:
食品安全
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分析化学
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2019
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IF 2.813
Tengfei Li,Bin Huang,Duo Li,Yantong Zhu,Li Ding,Chang Shu
In this work, we developed and validated the specific, sensitive and simple LC–MS/MS method for quantification of eslicarbazepine in human plasma. The analyte samples were prepared through a simple one-step protein precipitation method by acetonitrile . The chromatographic separation was operated on an economical Hanbon ODS-2 C18 column (150 mm × 2.1 mm, 10 μm) with isocratic elution using 10 mM ammonium acetate containing 0.01% formic acid and acetonitrile (72:28, v/v) as the mobile phase at the flow rate of 0.5 mL/min. The mass quantification was carried on the multiple reaction monitoring (MRM) of the transitions of m / z 255.1 → 194.1 for eslicarbazepine and m / z 446.1 → 321.1 for glipizide (the internal standard), respectively. The established method was validated with acceptable specificity, linearity, accuracy, precision, extraction recovery, matrix effect and stability in accordance with FDA regulations. At last, the validated method was successfully applied to determination of eslicarbazepine in human plasma obtained from clinical study.
研究领域:
药物分析
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临床药理学
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2023
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IF 3
Zheyue Bo,Wanjun Han,Haoyue Zhao,Han Liu,Ting Liang,Lanjing Li,Taotao Peng,Ying Li,Chunshan Gui
Cypate, a heptamethine cyanine dye, is a prototypic near-infrared (NIR) theranostic agent for optical imaging and photothermal therapy. In the present study, a selective, sensitive, and rapid liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the quantitation of cypate in mouse plasma. The chromatographic separation was achieved using a short C 18 column (2.1 mm × 50 mm, 5 μm) with a run time of 5 min. The MS was operated in multiple reaction monitoring (MRM) mode via positive electrospray ionization. The ion transitions for cypate and internal standard IR-820 were m / z 626.3 → 596.3 and m / z 827.4 → 330.2, respectively. The method was linear over a concentration range of 1.0–500 ng/mL. The within-run and between-run precision was less than 14.4% with accuracy in the range of −13.4% ∼ 9.8%. The validated method was successfully applied to a pharmacokinetic study of cypate in mice following intravenous administration.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2021
·
IF 3.935
Xinying He,Han Cao,Xia Li,Yan Li,Yunqiu Yu
Lysophosphatidylcholine (LPC) was commonly known as a class of significant differential metabolites of high relevance with many diseases including psoriasis, of which the accurate determination is of great importance to diagnosis or prediction to many diseases. However, it is challenging and complicated because of the enormous biological sample complexity and impurities interference. In this study, we synthesized a magnetic nanocomposite MG@PD@TiO 2 and took advantage of the interactions of Lewis acid−base between the phosphate groups in LPCs and Ti ions on MG@PD@TiO 2 nanomaterials for selective separation and enrichment of LPCs from complex biological matrix. The solid-phase extraction sample pretreatment process by means of MG@PD@TiO 2 nanomaterials coupled with LC–MS/MS method was then applied to actual determination of six typical LPCs (LPC 10:0, 14:0, 16:0, 18:0, 18:1, 22:0) in human plasma. The extraction conditions were scientifically optimized by single-factor test (adsorbent amount, adsorption and desorption time, elution solvent type, eluant volume). Under the optimal conditions, the detection limits (LOD, S/N = 3) and quantification limits (LOQ, S/N = 10) were 1 and 5 ng/mL for LPC 10:0 and LPC 14:0, 0.02 and 0.1 ng/mL for LPC 16:0 and LPC 18:1, 0.05 and 0.2 ng/mL LPC 18:0 and LPC 22:0, respectively. The intra- and inter-day precisions were 3.82–12.60 % (n = 6) and 3.29–13.50 % (n = 6) respectively, the recoveries were in the range of 91.92–113.69 % and the stability of the analytes in the matrix performed well with RSDs≤15.51 %. Finally, the developed method was successfully applied to the accurate determination of six LPCs biomarkers of plasma in patients with psoriasis (n = 10) and control groups (n = 10).
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FOOD AND AGRICULTURAL IMMUNOLOGY
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2021
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IF 3.101
Enhui Guo,Linchuan Zhao,Kang Wu,Wen Huang,Kang Zhao,Jianguo Li,Anping Deng
Amphenicol antibiotics including chloramphenicol (CAP), florfenicol (FF) and thiamphenicol (TAP) have been widely used in aquaculture and veterinary to treat various infections. Because of their high toxicity, it is important to detect these amphenicol antibiotics simultaneously. Using the monoclonal antibody against CAP (mAbCAP) binding CAP only and the mAbFF recognizing both FF and TAP, the two antibodies were covalently coupled to CNBr-activated Sepharose-4B for the simultaneous extraction of CAP, FF and TAP from samples. The bound CAP, FF and TAP were eluted from the Sepharose-4B and measured by LC–MS/MS. The extraction conditions of the two-antibodies-immobilized immunoaffinity clean-up (IAC) for CAP, FF and TAP were optimized and the maximum capacity was investigated. The extraction efficiency of IAC for CAP, FF and TAP was 1.1–2.1 times higher than that of SPE. The LC–MS/MS coupled with IAC was a powerful analytical method for the detection of CAP, FF and TAP simultaneously.
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INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES
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2024
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IF 7.7
Kewei Zheng,Yuanyuan Wu,Qingfei Dai,Xiaojun Yan,Yu Liu,Di Sun,Zhongjie Yu,Shuoqi Jiang,Qingbao Ma,Wei Jiang
The objective of this study was to explore the potential of Antarctic krill-derived peptides as α-glucosidase inhibitors for the treatment of type 2 diabetes. The enzymolysis conditions of α-glucosidase inhibitory peptides were optimized by response surface methodology (RSM), a statistical method that efficiently determines optimal conditions with a limited number of experiments. Gel chromatography and LC-MS/MS techniques were utilized to determine the molecular weight (M w ) distribution and sequences of the hydrolysates. The identification and analysis of the mechanism behind α-glucosidase inhibitory peptides were conducted through conventional and computer-assisted techniques. The binding affinities between peptides and α-glucosidase were further validated using BLI (biolayer interferometry) assay. The results revealed that hydrolysates generated by neutrase exhibited the highest α-glucosidase inhibition rate. Optimal conditions for hydrolysis were determined to be an enzyme concentration of 6 × 10 3 U/g, hydrolysis time of 5.4 h, and hydrolysis temperature of 45 °C. Four peptides (LPFQR, PSFD, PSFDF, VPFPR) with strong binding affinities to the active site of α-glucosidase, primarily through hydrogen bonding and hydrophobic interactions. This study highlights the prospective utility of Antarctic krill-derived peptides in curtailing α-glucosidase activity, offering a theoretical foundation for the development of novel α-glucosidase inhibitors and related functional foods to enhance diabetes management.
研究领域:
生物化学
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药理学
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食品科学
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糖尿病研究
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Pharmaceutics
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2024
·Vol. 16
·期 5
·591
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IF 4.9
Liang Wu,Danfeng Li,Peijing Wang,Linling Dong,Wang Zhang,Jianjun Xu,Xiaoliang Jin
Pedunculoside, a triterpene saponin derived from variousIlexspecies, holds potential as a treatment for cardiovascular diseases. However, its clinical application is hindered by poor bioavailability, rapid elimination, and extensive intestinal metabolism to rotundic acid. To address these issues, a water-soluble inclusion complex of pedunculoside, namely, the beta-CD polymer inclusion complex of pedunculoside (pedunculoside–βCDP), was prepared in this study, and a comparative in vitro stability and pharmacokinetic behavior study was performed between pedunculoside and pedunculoside–βCDP. Both pedunculoside and pedunculoside–βCDP exhibited the highest stability in simulated gastric fluid and simulated intestinal fluid but were readily metabolized when co-incubated withBifidobacterium adolescentisandBifidobacterium breve. An LC-MS/MS analytical method for the simultaneous determination of pedunculoside and rotundic acid in rat plasma was successfully established, validated, and applied to investigate the pharmacokinetic behavior after rats were intravenously administered with pedunculoside or pedunculoside–βCDP. The results indicated that pedunculoside–βCDP could significantly improve the pharmacokinetic profile of pedunculoside by increasing plasma exposure, retarding elimination, and reducing intestinal metabolism. This study enhances our understanding of pedunculoside–βCDP’s metabolic fate and pharmacokinetic properties and potentially advances its further research, development, and clinical application.
研究领域:
药理学
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药物递送系统
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分析化学
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心血管研究
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2025
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IF 3.1
Jiangbin Han,Lijuan Zhai,Jie Wang,Biying Dai,Huiyue Lu,Jiao Chen,Xiaoli Wang,Yuyu Wu,Wen Qian
Hetrombopag (Hengqu®) is an oral nonpeptide thrombopoietin receptor agonist for the treatment of thrombocytopenia and aplastic anemia. Research on the pharmacokinetic behavior is very important, but accurate quantification of metal-sensitive hetrombopag in biological specimens is a challenging analytical problem. In view of the presence of trace metals from a variety of sources, such as chromatographic system, containers, and the mass spectrometry spray needle, which can contribute to poor peak shape, tailing, and diminished recovery of compound. To ameliorate these problems, different solvent additives, mobile phase, containers and precipitant reagents were investigated to reduce the negative effects. In the present study, a robust, selective, and sensitive liquid chromatography–tandem mass spectrometry (LC-MS/MS) method for the determination of hetrombopag in dog plasma was developed based on the dual strategies: (1) 6 % perchloric acid in acetonitrile eliminates metal ion adsorption in storage containers, and (2) 0.01 % trifluoroacetic acid (TFA) in the mobile phase suppresses chelation in chromatographic systems. These two solvents are essential requirements for ensuring stable analytical signals. This method employed an InfinityLab Poroshell 120 EC-C18 column (4.6 ×50 mm, 2.7 μm, Agilent) with a gradient system comprising 0.01 % trifluoroacetic acid with 10 mM ammonium formate (phase A) and a mixture of H 2 O: methanol: isopropanol (1:10:10, v/v/v) containing 0.01 % trifluoroacetic acid and 10 mM ammonium formate (phase B). The column temperature of 50℃ and the addition of isopropanol were beneficial for the separation of interfering peaks and target analyte peaks in plasma. The method exhibits excellent linearity over 3 orders of magnitude. The method achieved a lower limit of quantification (LLOQ) of 0.10 ng/mL using only 50 μL of plasma, with precision (RSD ≤ 8.83 %) and accuracy (88.4–102.2 %) within acceptable limits. The method was applied to determine the plasma concentration of hetrombopag in eight male beagle dogs after each administration of three 2.5 mg hetrombopag tablets. The analytical methodology described in the present work should be useful in the future work aiming to establish a model relating metal-sensitive other compounds.
研究领域:
分析化学
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药代动力学
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生物分析
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质谱分析
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药物研发
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2024
·Vol. 416
·期 29
·7043-7062
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IF 3.8
Liu Wen-Ya,Xu Di,Meng Hui-Hui,Wang Cheng-Yao,Feng Xin,Wang Jun-Song
Cucurbitacin B (CuB) is a natural triterpenoid with diverse pharmacological effects including potent anticancer activity. However, its oral bioavailability is hampered by limited metabolism in vivo. We characterized CuB’s in vivo metabolism in rats to uncover bioactive metabolites retaining therapeutic potential, using a robust UHPLC-Q-TOF–MS/MS workflow. This workflow combined molecular networking, fragmentation filtering, and mass defect filtering to identify CuB metabolites in rat urine, plasma, and feces following oral administration. Thirteen metabolites were identified and seven were confirmed. Major phase I transformations involved hydrolysis, reduction, epoxidation, and amination. Phase II conjugation included cysteine, glutathione, glucuronide, and gluconic acid conjugates. Notably, one of the main metabolites formed was the cysteine conjugate CuB-Cys. CuB-Cys maintained similar in vitro antiproliferative activity to CuB on HepG2, MCF-7, and PANC-1 cancer cell lines. However, it demonstrated lower cytotoxicity towards non-cancerous L02 cells, highlighting improved therapeutic selectivity. Mechanistically, CuB-Cys induced greater apoptotic signaling in HepG2 cells than CuB via enhanced caspase activation and disrupted BAX-Bcl-2 balance. This represents the first systematic characterization of CuB’s in vivo metabolic pathway. The identification and confirmation of CuB-Cys provide insight for drug development efforts aiming to maintain therapeutic efficacy while reducing toxicity, via metabolite-based approaches. Our findings shed light on strategies for improving CuB’s clinical potential. Graphical Abstract
研究领域:
药理学
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代谢组学
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肿瘤学
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Toxicologie Analytique et Clinique
·
2025
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IF 1.7
Xiaolong Zhang,Kundi Zhao,Yuxuan Chen,Jinlei Liu,Jie Gu,Mengchao Wang,Yinyin Dai,Huimin Zhang,Amin Wurita,Koutaro Hasegawa
Summary Introduction Distribution of imidazole-derived GABA agonists, such as etomidate, metomidate and its analogs have been encountered frequently especially in China, along with its abuse cases. Recently, we were enquired to investigate urine samples and dubious powder seized from abuse cases, in which a new etomidate analog isopropoxate was detected. Methods The etomidate analog contained in the seized powder was tried to be identified using gas chromatography-mass spectrometry and by hydrolysis its ester structure to related alcohol under basic reaction environment, as a preliminary analysis for the powder composition. Reference standard were then purchased to identify the compound in suspected powder. For urine samples, after adding the internal standard and acetonitrile to the urine samples followed by vortexing and centrifugation, the supernatant layer was analyzed by LC-MS/MS. Results For LC-MS/MS analysis, the coefficient of determination (r2) values of the calibration curves of etomidate acid and isopropoxate in the urine were more than 0.99; the limits of detection (LODs) for etomidate acid, and isopropoxate was 0.025 ng/mL; the limits of quantification (LOQs) of them was 0.05 ng/mL. Etomidate acid and isopropoxate could be determined from submitted urines. And nine isopropoxate metabolites and their major metabolic pathways were identified. Conclusions In this study, we have established a simultaneous and reliable analytical method for etomidate acid and isopropoxate in human urine by LC-MS/MS, and the method could be applied to authentic cases. It is also the first time that the metabolic pathway of isopropoxate in the human body has been explored.
研究领域:
毒理学
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分析化学
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法医学
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CHROMATOGRAPHIA
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2024
·
IF 1.2
Han Kyoung-Moon,Woo In Suk,Park Chae Gyeong,Kim You Kyung,Yang Yoon Ji,Park Bo Reum,Choi Jang Duck,Son Kyung Hun
Preservatives can be used in natural and organic cosmetics to prevent quality deterioration during distribution and use, but the ingredients permitted are limited in the Republic of Korea. A method of simultaneous analysis was developed to monitor natural and organic cosmetics distributed online for the presence of 15 illegally used preservatives. Considering the complexities of the cosmetic matrices, an optimized sample preparation method is essential. Therefore, we developed the optimal purification method by comparing three preparation methods: QuEChERS, high-speed centrifugation, and solid-phase extraction (SPE). The SPE method, which exhibited the most favorable results in matrix reduction, was employed. To establish the SPE-ultra-high-performance liquid chromatography-diode array detection method, factors such as the mobile phase and column were optimized. The optimal separation of the 15 preservatives was observed under the following conditions: mobile phase A comprising 0.1% phosphoric acid in water with 0.5 mM sodium hexanesulfonate and a C 8 column (1.7 μm, 2.1 × 150 mm) as the stationary phase. The linear correlation coefficients were > 0.9998, and the limits of detection and quantitation ranged from 0.05 to 0.67 and 0.15 to 2.02 μg mL −1 , respectively. Using the established analytical method, illegally used preservatives were detected in products claimed to be natural and organic cosmetics sold on the market, and these findings were subsequently verified using liquid chromatography-tandem mass spectrometry. Six out of 47 samples contained phenoxyethanol and parabens. Therefore, this method will help manage the addition of illegal preservatives to natural and organic cosmetics.
研究领域:
分析化学
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化妆品科学
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高影响因子
危险品化学品经营许可证（带存储）