PREPARATIVE BIOCHEMISTRY & BIOTECHNOLOGY
·
2021
·
IF 2.162
Guilong Yan,Yuzhen Zhou,Yonghong Hu,Liqin Zhao,Wei Wang
Counter-current chromatography (CCC) target-guided by on-line HPLC with post-column DPPH assay was established for efficient screening and isolation of large amount of antioxidants from Eupatorium lindleyanum DC. On-line HPLC with post-column DPPH reaction was used to screen the antioxidants and optimize the biphasic solvent system of CCC, then the targeted peaks were purified using CCC. In the present study, three compounds, nepetin, cirsiliol and jaceosidin, were targeted and successively separated from n-butanol fraction of E. lindleyanum DC. by this strategy. All three compounds showed strong DPPH radical scavenging activity. These results confirmed that the strategy would be an efficient and effective method to isolate antioxidants from complex mixtures.
研究领域:
药用植物化学
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分离分析技术
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DOI
PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2023
·Vol. 415
·期 17
·3375-3384
·
IF 4.3
Liu Si,Lu Boling,Peng Zijuan,Liu Chunyu,Liu Yuhui,Jiao Hui,Wu Dan,Li Penghui,Zhao Xingchen,Song Shanjun
In organic purity assessment, chromatography separation with a suitable detector is required. Diode array detection (DAD) has been a widely used technique for high-performance liquid chromatography (HPLC) analyses, but its application is limited to compounds with sufficient UV chromophores. Charged aerosol detector (CAD), as a mass-dependent detector, is advantageous for providing a nearly uniform response for analytes, regardless of their structures. In this study, 11 non-volatile compounds with/without UV chromophores were analyzed by CAD using continuous direct injection mode. The RSDs of CAD responses were within 17%. For saccharides and bisphenols, especially, the RSDs were lower ( 2.12% and 8.14%, respectively). Since bisphenols exist in UV chromophores, their HPLC–DAD responses were studied and compared with CAD responses, with CAD showing a more uniform response. Besides, the key parameters of HPLC-CAD were optimized and the developed method was verified using a Certified Reference Material (CRM, dulcitol, GBW06144). The area normalization result of dulcitol measured by HPLC-CAD was 99.89% ± 0.02% ( n = 6), consistent with the certified value of 99.8% ± 0.2% ( k = 2). The result of this work indicated that the HPLC-CAD method could be a good complementary tool to traditional techniques for the purity assessment of organic compounds, especially for compounds lacking UV chromophores. Graphical Abstract
研究领域:
分析化学
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药物分析
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DOI
PubMed
高影响因子
TALANTA
·
2016
·
IF 4.035
Jiping Ma,Zhidan Yao,Liwei Hou,Wenhui Lu,Qipeng Yang,Jinhua Li,Lingxin Chen
Magnetic metal-organic frameworks (MOFs, [MIL-101]) were prepared and used as magnetic solid-phase extraction (MSPE) adsorbents for preconcentration of four kinds of pyrazole/pyrrole pesticides (flusilazole, fipronil , chlorfenapyr , and fenpyroximate) in environmental water samples, followed by high-performance liquid chromatography-diode-array detector (HPLC-DAD) determination. Several variables affecting MSPE efficiency were systematically investigated, including amount of MIL-101, extraction time, sample pH, salt concentration, type of desorption solvent and desorption number of times. Under optimized conditions, excellent linearity was achieved in the range of 5.0–200.0 μg/L for flusilazole and fipronil, and 2.0–200.0 μg/L for chlorfenapyr and fenpyroximate, with correlation coefficients r >0.9911. Limits of detection and quantification were 0.3–1.5 μg/L and 1.0–5.0 μg/L, respectively. The intra-day and inter-day precision (relative standard deviation, n =6, %) at three spiked levels were 1.1–5.4% and 3.9–7.8% in terms of peak area, respectively. The method recoveries at three fortified concentration levels ranged from 81.8% to 107.5% for reservoir water samples, 81.0–99.5% for river water samples, and 80.2–106.5% for seawater samples. The developed MOFs based MSPE coupled with HPLC method proved to be a convenient, rapid and eco-friendly alternative to the sensitive determination of pyrazole/pyrrole pesticides with high repeatability and excellent practical applicability.
研究领域:
环境科学
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分析化学
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DOI
PubMed
高影响因子
TALANTA
·
2019
·
IF 4.916
Yan Zhang,Donghao Liu,Jun Peng,Yanru Cui,Yi Shi,Hua He
A novel magnetic surface molecular imprinted polymers with 2, 4, 6-trisacrylamido-3, 5-triazine (TAT) as a functional monomer was successfully synthesized and used for the enrichment and determination of zearalenone . The molecular imprinting is reported herein at first time for application of zearalenone in wheat. The magnetic imprinted materials possessed excellent magnetism and uniform appearance, which were characterized by fourier transform infared spectroscopy and transmission electron microscope. The results proved the magnetic molecular imprinted polymers was successfully prepared. The magnetic molecular imprinted polymers exhibited satisfactory sensitivity, stability and potential reusability. The binding affinity was investigated by selectivity experiment, which possessed high selectivity. To obtain the optimal application conditions, the amount of adsorption, extraction time, elution solvent and time were optimized. The limited detection of zearalenone was 0.55 ng g −1 and the recoveries of zearalenone were 92.1–96.0%. The relative standard deviation was lower than 5.4%. This indicated that a simple, efficient and low-cost method was established and successfully applied in spiked wheat sample.
研究领域:
食品安全
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分析化学
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DOI
PubMed
高影响因子
RSC Advances
·
2019
·Vol. 9
·期 44
·25797-25804
·
IF 3.049
Shunli Ji,Hongbin Gao,Xingya Xia,Feng Zheng
Benzyl halides, widely used as alkylation reagents in drug synthesis, are potential genotoxic impurities (PGTIs) required to be controlled at trace levels. However, the existing analytical methods for benzyl halides often suffer from matrix interferences or low derivatization efficiency of benzyl chlorides. In this paper, a simple derivatization HPLC-UV method was developed for the analysis of these residual trace benzyl halides in drug substances. 1-(4-Nitrophenyl) piperazine (4-NPP) was selected as a new derivatization reagent because it shifted well the benzyl halides derivatives away to the near visible range (392 nm), which could minimize the matrix interferences from the drug substances and related impurities. Meanwhile, potassium iodide (KI) was used to convert the mixed benzyl halides into benzyl iodides before derivatization. The derivatization parameters were also optimized using the design of experiments (DoE) for achieving the best reaction efficiency. The results showed that the new approach had high specificity and sensitivity, and the LOQs were 7–9 μg g−1 relative to 5 mg mL−1 antipyrine and 17.5–22.5 μg g−1 relative to 2 mg mL−1 oroxylin A. The method is a valuable alternative for the determination of residual benzyl halides in the drug substances.
研究领域:
药物分析
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毒理学
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DOI
PubMed
高影响因子
Analytical Methods
·
2014
·Vol. 6
·期 5
·1563-1568
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IF 1.938
Huang Yang,Li Kang,Shao Hui Kai,Liu Sheng Quan,Xiang Fei Jun
A method using molecularly imprinted solid-phase extraction combined with RP-HPLC-UV was developed for determination of liquiritin (LQR) in rat plasma after oral administration of Compound Liquorice Tablets (CLTs). To this end, molecularly imprinted polymers were prepared by in situ polymerization, using LQR as the template, acrylamide as the functional monomer, and ethylene glycol dimethacrylate as the crosslinker, whose solid-phase extraction properties for liquiritin were evaluated by HPLC-UV. The enrichment and extraction recovery were investigated in the study after the extraction procedure was optimized. The recovery was larger than 85.0% and the RSD was less than 10.0%. The calibration curve was expressed as y = 16 004x − 1.864 (r = 0.996) with a linear range of 0.007–1.683 μg mL−1. Besides, the Tmax was 0.5 h for liquiritin and the Cmax was 0.8 μg mL−1 after oral administration of compound liquorice tablets. In addition, the pharmacokinetic parameters were calculated using a two-compartment model. The results indicated that the monolithic polymer pipette presented a good extraction efficiency for liquiritin. At the same time, the results indicated that the index components could basically reveal the pharmacokinetic behavior. This study was aimed to explore an approach that could be applied to promulgate the pharmacokinetics and provide more information for clinical applications.
研究领域:
药理学
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分析化学
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生物医学工程
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DOI
高影响因子
FOOD CHEMISTRY
·
2014
·
IF 3.259
Chanjuan Xu,Bingxian Yang,Wei Zhu,Ximin Li,Jingkui Tian,Lin Zhang
The leaves of Linderae aggregate (LAL) has been used as a type of tea in China and other Southeast Asian countries. In this study, 11 polyphenols in LAL were clarified for the first time using multiple high-performance liquid chromatographic techniques. An optimal extracting method was developed through the comparison of the amount of quercetin-3- O -α- l -rhamnoside using a uniform design method. From the fingerprint liquid chromatography data, 11 common peaks in the 8 samples collected from April to November were semi-determined. The antioxidant capacities were examined using the 2,2-diphenyl-1-picrylhydrazyl free radical scavenging assay and the ferric reducing/antioxidant power assay. All 8 samples contained the same 11 polyphenols in similar ratios. Three samples, S2, S5 and S6 contained higher amount of quercetin-3- O -α- l -rhamnoside and were demonstrated to have stronger antioxidant capacities in both antioxidant assays. These results are critical in optimising harvest time and quality control of LAL.
研究领域:
植物化学
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药理学
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分析化学
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DOI
高影响因子
Analytical Methods
·
2022
·Vol. 14
·期 25
·2531-2540
·
IF 3.532
Wenjing Li,Maoyu Cao,Pengxiang Ge,Xiaoyu Fu,Jiajie Tang,Mindong Chen
Organosulfates (OSs) derived from the oxidation of biogenic volatile organic compounds (BVOCs) in the presence of anthropogenic sulfate aerosols are the important tracers of secondary organic aerosols (SOAs). In order to better understand the concentration of pinene-nitrooxy organosulfates (pNOSs) in Nanjing, a sensitive high-performance liquid chromatography-electron spray ionization spectrum/mass spectrum (HPLC-ESI-MS/MS) to determine pNOSs in PM2.5 has been developed and validated in this study. Firstly, Hypersil Gold C18 (Thermo Scientific, San Jose, USA) was selected to separate pinene-derived nitrooxy organosulfates (pNOSs) based on their polarity. Three kinds of pNOSs were detected in the full scan mode (MS) with an ESI source under the negative mode. Secondly, three isomers of pNOSs with fragment ions m/z 220, 151, and 142 were identified based on the MS/MS maps. At least two pairs of transfer ions should be selected as identification and quantification ions according to the optimization results of target compounds. For example, to determine pNOSs, these transfer ions of m/z 294 → 247, m/z 294 → 231, m/z 294 → 220, m/z 294 → 142, m/z 294 → 151, m/z 294 → 96, m/z 294 → 80 were selected as quantification and identification ions. Finally, the influence of scan mode on pNOS detection was evaluated, and the results showed that pNOSs were most sensitive in the SRM (selected reaction monitor) scan mode. Therefore, the SRM scan mode was chosen to detect pNOSs. We applied this method to analyze year-round PM2.5 (PM2.5 is fine particulate matter, which refers to particulate matter in ambient air with an aerodynamic equivalent diameter of less than or equal to 2.5 microns) samples in Nanjing. The average concentration of all the three kinds of pNOSs was 69.95 ng m−3. The results showed that the average concentration of pNOSs was high in spring (92.94 ng m−3) and summer (90.57 ng m−3), and lowest in winter (30.03 ng m−3).
研究领域:
大气化学
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环境科学
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分析化学
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DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2024
·
IF 1.8
Yonglin Ma,Yue Zhang,Yu Zhao,Jiwen Wang,Qianqian Hu,Lianlin Yang,Shuzhen Chen,Yong Diao,Hongliang Ma
In this study, an online antioxidant assay based on HPLC-ABTS was mainly developed for screening the antioxidants of flavonoids from Astragali Radix (AR), and comparing the antioxidant capacity between traditional decoction pieces (TDP) of AR and cell wall-broken decoction pieces (CDP) of AR. The experimental results showed that the overall antioxidant capacity of CDP of AR was about twice as much as that of TDP of AR, which was specifically expressed as the antioxidant capacity of the screened antioxidants extracted from CDP was equivalent to 1.9–5.1 times that of those extracted from TDP, and three antioxidants were successfully screened, which were calycosin-7-O-β-D-glucoside, calycosin, and formononetin. The method established in this study is characterized by high efficiency and accuracy, which can simultaneously accomplish the screening of antioxidant components and the comparison of antioxidant capacity between samples, and provides a new method for the quality evaluation of AR from the perspective of antioxidant activity.
研究领域:
中药学
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分析化学
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产品关联
DOI
PubMed
高影响因子
Canadian Journal of Chemistry
·
2013
·Vol. 91
·期 11
·
IF 0.964
ChenMiao,LiuLiangliang,ChenXiaoqing
Alcohol dehydrogenase (ADH) is a key enzyme that converts ethanol into acetaldehyde. Its binders could be used to efficiently treat human toxic alcohol poisoning and suppress the acetaldehyde accumulation in alcohol hypersensitive alcoholics. In the present study, a new assay based on ADH-functionalized magnetic nanoparticles coupled with high-performance liquid chromatography − tandem mass spectrometry (HPLC−MS/MS) was developed for the rapid screening and identification of ADH binders. ADH was immobilized on silica-coated Fe3O4 magnetic nanoparticles via covalent bonds and the synthesized nanoparticles were characterized by TEM, XRD, FT-IR, and VSM. The amount of bound ADH onto magnetic nanoparticles was 80.6 μg/mg. The optimum temperature and pH for the enzymatic activity of immobilized ADH were 25 °C and 7.0, respectively. The relative activity of immobilized ADH remained 68.14% after 10 times of recycle, which exhibited good durability. Nine compounds with ADH-binding activity were screened and identified in Glycyrrhiza uralensis root extracts, among which seven compounds were first screened and identified. Experimental results proved that the proposed method could rapidly screen ADH binders from complex mixtures.
研究领域:
生物化学
·
药物开发
·
分析化学
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DOI
高影响因子
TALANTA
·
2025
·
IF 6.1
Zheng Hu,Yuhang Yang,Zhe Li,Qiuying Tao,Yinghong Huang,Xian Wang
Endocrine-disrupting chemicals (EDCs) are a growing class of pollutants commonly found in environmental matrices due to their extensive use in pharmaceuticals and personal care products (PPCPs). In this study, a novel magnetic covalent organic framework (COF), Fe 3 O 4 –COOH@TFP-BHBD, was successfully synthesized and utilized as an adsorbent for magnetic solid-phase extraction (MSPE) of EDCs from PPCPs. The core-shell structured adsorbent demonstrated a high specific surface area, strong magnetic responsiveness and excellent stability. A COF-MSPE-high-performance liquid chromatography-tandem mass spectrometry (COF-MSPE-HPLC-MS/MS) method was developed for the quantitative analysis of EDCs in PPCPs. Under the optimized condition, the detection and quantification limits of this method reached as low as 0.001–0.007 ng/mL and 0.004–0.025 ng/mL, respectively. This method was validated and proven capable to analyze real PPCP samples, while the spiked recovery rates in ranged from 85.62 to 107.83 % with RSD of 2.28–8.58 %. Moreover, the adsorption mechanism was investigated using density functional theory (DFT) calculations. The DFT results revealed that the efficient enrichment capacity of Fe 3 O 4 –COOH@TFP-BHBD for EDCs can be attributed to π-π interactions and hydrogen bondings. This proposed method provides excellent adsorption ability and sensitivity for the extraction and precise detection of EDCs in PPCPs.
研究领域:
环境科学
·
分析化学
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产品关联
DOI
PubMed
高影响因子
ANALYTICAL LETTERS
·
2022
·
IF 2.267
Ru Li,Xuan Zou,Pan Luan,Xiaokun Liu,Ning Wang,Qian Wang,Huashi Guan,Zhe Xu
Thrombosis is the main cause of many cardiovascular diseases. The conventional pharmaceuticals used for preventing thrombosis can induce significant adverse side effects, especially bleeding risk. Hence, the development of more effective and safe antithrombotic agents is strongly demanded to improve clinical treatment. In order to rapidly screen and identify novel antithrombotic substances from natural marine products, a multi-target screening strategy is reported to quantify the antithrombotic activity with high-performance liquid chromatography – mass spectrometry (HPLC-MS). Five key thrombosis-related targets, including thrombin, coagulation factors Xa, XIa and XIIa and platelet phosphodiesterase 3, were selected to establish the multi-target antithrombotic activity screening assay. The Michaelis-Menten constants (Km) were 8.16 µM, 58.85 µM, 120.03 µM, 35.24 µM and 79.67 µM, respectively. Five known inhibitors, namely argatroban, rivaroxaban, benzamidine, 3-carboxamide-coumarinand, and milrinone, were used for validation. The reproducibility of the screening strategy was verified by calculating the overall average Z′ value, which was 0.88. Subsequently, this method was assessed by screening a small marine library of 78 compounds. Five coumarin compounds were selected, and their antithrombotic activities were further validated in standard assessments of enzyme inhibition and on the coagulometer. According to the validation, the multi-target assay based on dried blood spots and HPLC-MS was suitable for screening antithrombotic substances with considerable reliability.
研究领域:
药理学
·
分析化学
·
心血管病学
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产品关联
DOI
高影响因子
危险品化学品经营许可证（带存储）