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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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2023
·
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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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.
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2019
·
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.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2018
·
IF 2.831
Renjie Hui,Yueying Gao,Jingyi Liu,Haili Liu,Chunlei Tang,Bainian Feng
Heart failure (HF) is one of the most serious health problems worldwide. A new positive inotropic compound, an isonicotinylhydrazide derivative (AF-HF001) was designed recently. A liquid chromatography-tandem mass spectrometry (LC–MS/MS) method was developed for the determination of the target analyte in mouse plasma. Samples were prepared by one step precipitation with ethyl acetate and stored in acetonitrile. Chromatographic analysis was carried out on a Hypersil Gold C 18 column (2.1 mm × 50 mm, 3 μm) with a gradient mobile phase consisting of acetonitrile and 0.1% aqueous formic acid. The analyte was detected by selective reaction monitoring (SRM) mode with target quantitative ion pair of m/z 292.1 → 148.2, using praziquantel as the internal standard (IS) m/z 313.1 → 203.2. Good linearity ( r = 0.995) was observed over a wide concentration range. The validation of method showed acceptable recovery and precision. The method has been then applied to a very first pharmacokinetic assay of AF-HF001 in mice.
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FOOD CHEMISTRY
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2022
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IF 9.231
Yuan-Yuan Zhang,Peng Zhang,Miao-Miao Le,Yan Qi,Zi Yang,Feng-Lin Hu,Tie-Jun Ling,Guan-Hu Bao
Cordyceps militaris ( C. militaris ) has been approved and widely used in healthy food. The present study aimed to improve the flavor of summer Keemun black tea (KBT) using C. militaris solid-state fermentation. Combined with sensory evaluation, the volatile and non-volatile components of solid-state fermentation of KBT (SSF-KBT) and KBT were analyzed. The results showed that after the solid-state fermentation, the contents of total polyphenol, total flavonoid, and total free amino acids were significantly reduced. Further non-targeted metabolomics analysis revealed that the contents of non-galloylated catechins and d -mannitol increased, while the galloylated catechins and flavonoid glycosides decreased as did the bitterness and astringency of KBT. Dihydro- β -ionone and β -ionone (OAV = 59321.97 and 8154.17) were the aroma-active compounds imparting woody and floral odors in SSF-KBT, respectively. Current study provides a new avenue to develop summer-autumn KBT.
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Food & Function
·
2022
·Vol. 13
·期 17
·9119-9142
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IF 6.317
Xiang Li,Yan Du,Chengping Zhang,Zhaoxin Tu,Li Wang
Highland barley (HB) displays a series of properties including regulation of lipid metabolism and attenuation of liver injury. Our study aimed to investigate the effect of modified highland barley (MHB) including fluidized highland barley (HB-1), extruded and puffed highland barley (HB-2), and ultrafine pulverized highland barley (HB-3) on lipid metabolism, liver inflammation, gut microbiota and metabolite profiles in mice fed with a high-fat/cholesterol diet (HFCD). 6 treatment groups were fed a normal control diet or an HFCD with or without MHB supplementation for 10 weeks. Results showed that MHB significantly improved lipid parameters, liver function and injury and blood glucose indexes related to hyperlipidemia compared with the HFCD group. In addition, MHB recovered the disorder of gut microbiota by increasing the Bacteroidetes/Firmicutes ratio and Lactobacillus and Allobaculum abundances and decreasing Proteobacteria abundance related to lipid metabolism bacteria. MHB reversed the decrease of short-chain fatty acid levels caused by the HFCD. Fecal metabolomics analysis showed that the important differential metabolites between HB-1 and HFCD were deoxycholic acid, myclobutanil and dibutyl phthalate, and the important differential metabolic pathways were arachidonic acid metabolism, ABC transporters and biosynthesis of unsaturated fatty acids. Results suggested that MHB especially HB-1 were better effective dietary intervention candidates to ameliorate hyperlipidemia compared with HB.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
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
·
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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BIOMEDICAL CHROMATOGRAPHY
·
2020
·Vol. 34
·期 8
·e4852
·
IF 1.728
Jing Wang,Yong Zhang,Meiqi Zhou,Meizhu Zheng,Jing Cui,Zhiqiang Liu,Chunming Liu,Shu Liu
Superoxide anion radical scavenger and xanthine oxidase inhibitor play an important role in the treatment of several relevant human diseases. In the present study, ultrafiltration liquid chromatography–mass spectrometry coupled to microplate reader was applied to screen and identify superoxide anion radical scavengers and xanthine oxidase inhibitors from total flavonoids of Ginkgo biloba leaves. As a result, four compounds (quercetin, apigenin, kaempferol and isorhamnetin) were screened as xanthine oxidase inhibitors by ultrafiltration LC–MS, and the 50% scavenging concentration values of the screened flavonoids were lower than those for allopurinol. Lineweaver–Burk plot results indicated that kaempferol was a competitive xanthine oxidase inhibitor; the other flavonoids were all anticompetitive inhibitors. Four flavonoids—rutin, quercetin, kaempferol and isorhamnetin—were screened as superoxide anion radical scavengers by LC–MS. The results demonstrate that the method for screening and evaluation of superoxide anion radical scavenger and xanthine oxidase inhibitor from a complex mixture system is feasible and efficient.
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Theranostics
·
2017
·
IF 8.766
Feifei Xu,Weixian Zhou,Jianxiang Cao,Qingqing Xu,Dechen Jiang,Yun Chen
The distorted and unique expression of microRNAs (miRNAs) in cancer makes them an attractive source of biomarker. There is much evidence indicating that a panel of miRNAs, termed “miRNA fingerprints”, is more specific and informative than an individual miRNA as biomarker. Thus, multiplex assays for simultaneous quantification of multiple miRNAs could be more potent in clinical practice. However, current available assays normally require pre-enrichment, amplification and labeling steps, and most of them are semi-quantitative or lack of multiplexing capability. In this study, we developed a quasi-targeted proteomics assay for multiplexed miRNA quantification by a combination of DNA-peptide probes and liquid chromatography-tandem mass spectrometry (LC-MS/MS). Specifically, the signal of target miRNAs (i.e., miR-21, miR-let7a, miR-200c, miR-125a and miR-15b) was converted into the mass response of reporter peptides by hybridization of miRNAs with DNA-peptide probes and subsequent tryptic digestion to release the peptides. After a careful optimization of conditions related to binding, conjugation, hybridization and multiple reaction monitoring (MRM) detection, the assay was validated for each miRNA and the limit of quantification (LOQ) for all the miRNAs can achieve 1 pM. Moreover, crosstalk between DNA-peptide probes in multiplex assay was sophisticatedly evaluated. Using this quasi-targeted proteomics assay, the level of target miRNAs was determined in 3 human breast cell lines and 36 matched pairs of breast tissue samples. Finally, simplex assay and qRT-PCR were also performed for a comparison. This approach grafts the strategy of targeted proteomics into miRNA quantification and may offer a new way for multiplexed miRNA profiling.
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MATERIALS RESEARCH BULLETIN
·
2025
·
IF 5.7
Ying Li,Huaping Xiong,Wei Shi,Zheming Ni,Shengjie Xia
Defect engineering and heterostructure construction are important strategies to enhance the photocatalytic performance of single-phase materials. In this study, an O- and Cd-dual-defect-modified LaOCl@CdS heterojunction (Ov-L@Cdv-C) was successfully constructed. Under visible light irradiation, using the typical fluoroquinolone antibiotic ciprofloxacin (CIP) as the target pollutant, Ov-L@Cdv-C exhibited superior photocatalytic degradation performance compared to Ov-LaOCl and Ov-L@CdS. Under optimal conditions (0.5 g/L catalyst, 0.010 g/L initial CIP concentration, pH = 5), the degradation efficiency of CIP reached 84.79 % within 150 min, significantly higher than that of Ov-LaOCl (48.73 %) and Ov-L@CdS (71.96 %). XPS and EPR characterizations confirmed the presence of abundant O and Cd dual defects in the Ov-L@Cdv-C heterojunction. ESR and free radical quenching experiments revealed that the main reactive species during the degradation process were ·O 2 − and h⁺. Based on work function calculations and built-in electric field analysis, a Z-scheme photocatalytic mechanism for the Ov-L@Cdv-C dual-defect heterojunction was proposed. Furthermore, LC-MS analysis identified the degradation intermediates and proposed three possible degradation pathways. In addition, T.E.S.T. predictions indicated that the toxicity of CIP gradually decreased during the photocatalytic degradation process.
研究领域:
环境科学
·
催化
·
材料科学
·
化学工程
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光化学
·
分析化学
·
毒理学
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