MICROCHEMICAL JOURNAL
·
2024
·
IF 4.9
Wenxu Hu,Yang Yu,Zhehui Weng,Yao Huang,Yanni Li,Dandan Ge
In this study, a new vortex-assisted dispersive liquid–liquid microextraction technique based on supramolecular solvent (SUPRAS) was proposed for the simultaneous extraction and preconcentration of aristolochic acids (AAs) in Aristolochia debilis followed by HPLC-DAD. A new type of SUPRAS, based on hexafluoroisopropanol (HFIP) and primary amine, with a higher density than water was prepared for the first time. HFIP acted as the coacervation agent and density modifier for the preparation of SUPRAS, and only a small amount of HFIP was required to form the SUPRAS. The influencing parameters such as the type and content of primary amine, the content of HFIP, vortex time, solution pH and ionic strength were thoroughly investigated and optimized. The prepared SUPRAS can effectively exclude macromolecules such as starch and be used to extract AAs from herbal medicines with high extraction efficiency. Under the optimized conditions, the method provided satisfactory linearity (1 ∼ 1000 ng mL −1 for AAb and 10 ∼ 1000 ng mL −1 for AAa with determination coefficients higher than 0.9981), low limits of detection (0.3 ∼ 3.1 ng mL −1 ) and limits of quantification (1.0 ∼ 9.5 ng mL −1 ). In addition, the intra-day and inter-day precision with relative standard deviations (RSDs%) below 6.8 % were obtained. Finally, the proposed method was applied to determine the AAs in Aristolochia debilis , the extraction recoveries were between 92.8 %∼100.6 % with RSDs% between 0.5 % and 7.2 %. Therefore, the developed method was an easy, efficient and reliable method for determining AAs in Aristolochia herbal materials.
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高影响因子
JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES
·
2025
·
IF 1.2
Ou Sha,Yuan Xu,Yunfan Wu,Dewei Wang,Yang Yao,Kaixuan Zhang
A magnetic graphene oxide/chitosan composite (MGO@CS) was synthesized via mechanochemistry and applied as an adsorbent for magnetic solid-phase extraction of four fluoroquinolone antibiotics in environmental water, prior to HPLC-fluorescence detection. Characterization confirmed the composite structure, and MSPE parameters were optimized. Results showed chitosan incorporation significantly improved elution efficiency. The adsorbent demonstrated reusability for six cycles. Under optimal conditions, the method demonstrated excellent linearity (1.0 × 10−4–2.0 × 10−1 mg/L, R2 ≥ 0.9990), with detection limits of 6.4 × 10−5–5.7 × 10−3 mg/L and quantification limits of 2.7 × 10−4–3.2 × 10−2 mg/L. Analysis of spiked environmental water samples yielded recoveries of 82.1–100.4% with relative standard deviations (RSDs) of 1.2–8.6%. These findings indicate that the proposed method is both effective and economical for the analysis of fluoroquinolone antibiotics in environmental water samples.
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DOI
高影响因子
TALANTA
·
2025
·
IF 6.1
Manyan Qiu,Aiai Nie,Jinghang Zhang,Miao Zheng,Ning Guan,Sharuna De,Xiaoyan Pei,Xinyan Yang,Yujun Jiang,Qianyu Zhao,Chaoxin Man
The effective separation of fat-soluble vitamins from complex matrices prior to instrumental analysis remains a significant challenge. Herein, a novel magnetic covalent organic framework (Fe 3 O 4 @tetrakis(4-aminophenyl)methane (TAM)-2,6-dihydroxynaphthalene-1,5-dicarbaldehyde (DHNDA), Fe 3 O 4 @TAM-DHNDA) was successfully designed and prepared for the efficient separation and enrichment of three fat-soluble vitamins in dairy products. The maximal adsorption efficiency of Fe 3 O 4 @TAM-DHNDA to fat-soluble vitamin was as high as 26.94 mg/g. Moreover, the adsorption mechanism of Fe 3 O 4 @TAM-DHNDA for V A , V D , and V E was revealed by molecular simulation techniques. Van der Waals forces and hydrogen bonds were the main interactions between Fe 3 O 4 @TAM-DHNDA and fat-soluble vitamins. Importantly, the magnetic solid phase extraction (MSPE) method based on Fe 3 O 4 @TAM-DHNDA could be used as an effective sample pretreatment technology for separation and enrichment of fat-soluble vitamins from complex matrices prior to instrumental analysis. When coupled with high-performance liquid chromatography-ultraviolet detector (HPLC-UV), the proposed method enables the efficient detection of fat-soluble vitamins in dairy products. The limit of detection (S/N = 3) and limit of quantification (S/N = 10) were achieved at 20–50 ng/mL and 55–150 ng/mL, respectively. Good linearity (R 2 > 0.9998) was obtained within the range of 2–100 μg/mL. The average recoveries of spiked milk samples were determined to be 83%–101% and the relative standard deviation (RSD) was 0.83% to 3.46% ( n =3). This work provides novel insights into the development of novel magnetic adsorbents and the separation and enrichment of fat-soluble vitamins in complex matrices.
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DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Yuejiao Yang,Xitian Peng,Guiyou Chen,Huaming Xiao,Qiongwei Yu
Perfluorinated compounds (PFCs) are persistent in urban water systems, threatening the safety of drinking water and aquatic food chains. In this study, fluorinated loofah sponge (FLS) was prepared for selective solid-phase extraction (SPE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) determination of 16 PFCs in urban water. The limits of detection (LODs) and limits of quantification (LOQs) of the established method (FLS-based SPE-LC-MS/MS) were 0.006–5 ng/mL and 0.01–10 ng/mL, respectively. This method exhibited a desirable precision with relative standard deviations (RSDs) less than 8.83 % and recoveries in the range of 85.4 %–107.2 %. Finally, this method was successfully applied to investigate the distribution of 16 PFCs in real urban water samples (such as tap water, bottled water, and lake water) collected in Wuhan, China, which enables sensitive dynamic monitoring of PFC migration in urban water networks and identification of potential sources so as to safeguard drinking water quality against emerging PFC contamination.
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高影响因子
FOOD CHEMISTRY
·
2024
·
IF 8.5
Jie Shi,Mingquan Huang,Qiang Yang,Yin Xu,Jihong Wu,Hongqin Liu,Jinglin Zhang,Fuping Zheng,Wei Dong
A new convenient method for identifying colorant compounds (CCs) in food matrices was developed using high-performance liquid chromatography with a diode array detector and quadrupole-time-of-flight mass spectrometer (HPLC-DAD-Q/TOF-MS) combined with theoretical calculations. A model sample containing three typical CCs was completely separated via HPLC-DAD. The obtained 3D ultraviolet-visible (UV–vis) spectra revealed the maximum absorption wavelengths (MAWs) of all CCs (yellow, 430 nm; red, 520 nm; blue, 620 nm) in the range of 400–800 nm, and their colors were determined based on their MAWs. Temporary structures of the CCs were obtained using Q/TOF-MS analysis. Theoretical calculations were then performed to obtain the theoretical MAWs and colors of the CCs according to their calculated UV–vis spectra based on temporary structures. The structures of the CCs were confirmed without the need for authoritative standards by comparing the consistency between their experimental and theoretical MAWs and colors. This method is particularly suitable for identifying CCs or compounds with UV–Vis absorption, including new compounds, compounds for which standards are difficult to obtain, and known compounds without reporting relevant molecular information.
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DOI
PubMed
高影响因子
ACS Applied Polymer Materials
·
2024
·
IF 4.4
Qinghai Hu,Lanling Chu,Yuqi Dai,Lanmei Zhang,Xuejun Kang,Xinming Wang
The efficient solid-phase extraction (SPE) adsorbents for the detection of trace mycotoxins are challenging to prepare in an essential sample pretreatment. In this study, an efficient SPE adsorbent, an electrospun polystyrene/polyacrylonitrile nanofiber membrane modified by polydopamine (PDA@PS/PAN NFM), was prepared and characterized. It is shown that the introduction of PDA provided abundant amino groups and phenolic hydroxyl groups for the porous network structure of these nanofibers, which can contribute rich interactions (such as hydrogen bonding, electrostatic interaction, and π–π stacking) on the analyte to improve the extraction efficiency of sample pretreatment. The extraction performance of PDA@PS/PAN NFM was probed by selecting zearalenone (ZEN) as the representative mycotoxin, and the effects of several factors on the adsorption and desorption in the SPE process were systematically investigated and optimized. Under the optimal conditions, the limit of detection (LOD) was 4.17 μg/kg, the intraday and interday relative standard deviations (RSDs) were 3.3–5.2 and 3.7–5.1%, respectively, and the recovery was 87.3–99.5%. Additionally, PDA@PS/PAN NFM displayed excellent reproducibility with a good reusability of 20 times. The results indicated that the PDA-functionalized nanofiber membrane exhibited extensive application prospects in the efficient separation, preconcentration, and decrease of interference of trace mycotoxins in a complex sample matrix.
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高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2021
·
IF 3.205
Dandan Wang,Rui Liu,Jinxiang Zeng,Chunhu Li,Wei Xiang,Guoyue Zhong,Zhining Xia
An in vitro intestinal absorption model combined with high-performance liquid chromatography-photo diode array-tandem mass spectrometry (HPLC-PDA-MS) was used for preliminary screening of potential active ingredients from complex multi-component traditional Chinese medicine (TCM) system. Oral administration is one of the main administration methods for TCMs. Only the ingredients that could be absorbed have the opportunity to play a role. Thus, these were defined as potential active ingredients. Studying of intestinal absorption can provide a theoretical basis for the mechanism of TCMs. The Caco-2 cell model, the everted rat gut sac model, and the Ussing chamber model were established for TCMs. The degree of anastomosis between the in vitro intestinal model and the actual intestinal absorption of TCMs were evaluated by the gavage method in rats. The Ussing chamber model was best fit for oral experiments in rats and was selected as the research means to preliminarily screen potential active ingredients from eight TCMs, including Salvia miltiorrhiza Bunge, Astragalus propinquus Schischkin, Plantago asiatica L , Fallopia multiflora (Thunb.) Harald, Epimedium brevicornu Maxim, Moutan Cortex , Citrus reticulata Blanco , and Panax notoginseng (Burkill) F. H. Chen ex C. H. Chow. A total of 44 components were absorbed and screened as the potential active ingredients from the 80 components identified in eight TCMs by HPLC-PDA-MS.
研究领域:
药理学
·
分析化学
·
传统医学
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DOI
PubMed
高影响因子
Analytical Methods
·
2013
·Vol. 6
·期 1
·194-201
·
IF 1.855
Ke-Jing Huang,Yu-Jie Liu,Jing Li,Tian Gan,Yan-Ming Liu
A graphene (Gr) functionalized silica gel (Gr–SiO2) sorbent was prepared and used as a new sorbent for solid-phase extraction (SPE) of polycyclic aromatic hydrocarbons (PAHs) including naphthalene, acenaphthylene, fluorene, phenanthrene, fluoranthene, and pyrene. The analytes were separated and detected by high-performance liquid chromatography (HPLC) with a UV detector. Factors affecting the extraction efficiency including the eluent type and its volume, adsorbent amount, sample volume, sample pH and flow rate were optimized. Under the optimized conditions, the present method showed a wide linear range (0.01–600 μg L−1), acceptable repeatability of the extraction (RSDs of 1.7–8.2%, n = 3) and satisfactory detection limits (0.0029–0.052 μg L−1). The recovery studies using this new sorbent were performed by three consecutive extraction steps of water and milk samples at three spiked levels. The average recoveries of the analytes in environmental water and milk samples were 89.0–115.4%, which demonstrated the applicability of the developed method.
研究领域:
分析化学
·
环境科学
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高影响因子
Asian Journal of Pharmaceutical Sciences
·
2016
·Vol. 12
·期 2
·202-208
·
IF 0
Huiyan Shi,Chenzhi Hou,Liqiang Gu,Zhe Wei,Hang Xing,Meiyu Zhang,Shixiao Wang,Longshan Zhao,Kaishun Bi,Xiaohui Chen
The present study was designed to investigate the influence of the pretreatment of piperazine ferulate on pharmacokinetic parameters of methotrexate in methotrexate-induced renal injury rats. A simple and efficient high performance liquid chromatography coupled with mass spectrometry (HPLC-MS) method was developed to determine methotrexate in rat plasma. Methotrexate and syringic acid (internal standard) were extracted from rat plasma samples by protein precipitation with acetonitrile. The analysis was performed on a CAPCELL PAK C 18 column (150 mm × 4.6 mm, 5 µm) with acetonitrile and 5 mmol/l ammonium acetate aqueous (10:90, v/v ). The linear range was 5.0 × 10 −2 to 100.0 µg/ml for methotrexate. Other parameters were all within the acceptance criteria. The validated method was successfully applied the pharmacokinetic study of methotrexate between two methotrexate treated groups (with and without the pretreatment of piperazine ferulate). Compared with the methotrexate treated alone group, the pharmacokinetic parameters in the methotrexate with the pretreatment of piperazine ferulate group showed significantly lower MRT (0-t) , MRT (0-∞) and T 1/2 . Results suggested that methotrexate can be rapidly eliminated, cleared or metabolized in rat blood, which might be related to the pretreatment of piperazine ferulate. The method provided deeper insights into rational clinical use of methotrexate with the pretreatment of piperazine ferulate on cancer patients with renal dysfunction.
研究领域:
药理学
·
药物代谢
·
肾脏病学
·
肿瘤学
·
临床药学
·
分析化学
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DOI
BIOMEDICAL CHROMATOGRAPHY
·
2014
·Vol. 29
·期 6
·869-875
·
IF 1.662
Yonggang Chen,Junhua Meng,Jili Zou,Jing An
Hordenine is an active compound found in several foods, herbs and beer. In this work, a novel sorbent was fabricated for selective solid-phase extraction (SPE) of hordenine in biological samples. The organic polymer sorbent was synthesized in one step in the plastic barrel of a syringe by a pre-polymerization solution consisting of methacrylic acid (MAA), 4-vinylphenylboronic acid (VB) and ethylene glycol dimethacrylate (EGDMA). The conditions for preparation were optimized to generate a poly(MAA-VB-EGMDA) monolith with good permeability. The monolith exhibited good enrichment efficiency towards hordenine. By using tyramine as the internal standard, a poly(MAA-VB-EGMDA)-based SPE-HPLC method was established for analysis of hordenine. Conditions for SPE, including volume of eluting solvent, pH of sample solution, sampling rate and sample volume, were optimized. The proposed SPE-HPLC method presented good linearity ( R 2 = 0.9992) within 10–2000 ng/mL and the detection limits was 3 ng/mL, which is significantly more sensitive than reported methods. The method was also applied in plasma and urine samples; good capability of removing matrices was observed, while hordenine in low content was well extracted and enriched. The recoveries were from 90.6 to 94.7% and from 89.3 to 91.5% for the spiked plasma and urine samples, respectively, with the relative standard deviations <4.7%. Copyright © 2014 John Wiley & Sons, Ltd.
研究领域:
分析化学
·
生物分析
·
分离科学
·
药物分析
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高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2017
·Vol. 40
·期 15
·3074-3085
·
IF 2.557
Lingfei Han,Desheng Hou,Congyu Ma,Na Fu,Jing Liu,Feng Feng,Wenyuan Liu,Feng Zheng
Short-chain aliphatic amines are a class of hazardous impurities in drug substances. A simple method, involving derivatization followed by high-performance liquid chromatography with diode array detection, has been developed for residue determination of eight aliphatic amines simultaneously in drug substances. Different halonitrobenzenes derivatization reagents were systematically compared. As a result, 1-fluoro-2-nitro-4-(trifluoromethyl)benzene was selected since the derivatization effectively shifted the absorption wavelength to the visible region (400–450 nm), where most drug substances, impurities and even the derivatization reagent absorb very weakly. Due to the redshift effect, interference was minimized and adequately low limits of quantitation were reached (0.24–0.80 nmol/mL). Moreover, the derivatization reaction was readily carried out in dimethyl sulfoxide at room temperature for 1 h using N , N -diisopropylethylamine as catalyst to achieve the highest yield. Without any pre-treatment, the derivatives were analyzed by high-performance liquid chromatography with diode array detection. The high stability of the derivatives within 24 h at room temperature (RSD<1.04%) further facilitated the simultaneous preparation and consecutive analysis of quantities of samples. Finally, the proposed method was successfully applied for residue determination of eight aliphatic amines simultaneously in eight drug substance samples. This study could be helpful for the routine analysis and residue control of aliphatic amines in drug substances.
研究领域:
药物分析
·
分析化学
·
杂质谱分析
·
色谱学
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高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2022
·Vol. 45
·期 11
·1847-1855
·
IF 3.614
Ben Chen,Haibo You,Liqun Fang,Tingting Lin,Ping Xu,Chu Chu,Shengqiang Tong
Analytical enantioseparations of five N-alkyl drugs, fluoxetine hydrochloride, labetalol, venlafaxine hydrochloride, trans -paroxol, and atropine sulfate, were investigated by reverse phase high-performance liquid chromatography with sulfobutylether-β-cyclodextrin as chiral mobile phase additive. Effects of various factors such as composition of mobile phase, concentration of cyclodextrins, and column temperature on retention and enantioselectivity were studied. Apparent formation constant between methanol, acetonitrile, and sulfobutylether-β-cyclodextrin were determined to be 2.90 × 10 −3 and 1.00 × 10 −4 L mmol −1 under 25°C using UV-spectrophotometry. Van't Hoff plots were used to investigate thermodynamic parameters for enantiomers–stationary phase interaction and formation of inclusion complex. Two retention models were employed individually for evaluation of inclusion complexation between five racemates and sulfobutylether-β-cyclodextrin. The second model with complex adsorption was more accord with the retention behavior of fluoxetine hydrochloride, labetalol, and venlafaxine hydrochloride enantiomers, while the first model was more consistent with the retention behaviors of trans -paroxol and atropine sulfate. In the selected mobile phase, stoichiometric ratio for both of inclusion complex was found to be 1:1.
研究领域:
药学
·
分析化学
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高影响因子
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