JOURNAL OF CHROMATOGRAPHY A
·
2026
·
IF 4
Jiaoqing Wei,Jiajia Wu,Xiaowen Hou,Rong Wang,Zhengyi Chen
A heat-assisted array gas membrane separation strategy coupled with High-Performance Liquid Chromatography Fluorescence detection was developed for sensitive determination of metformin based on an indirect quantification principle. Metformin was converted in situ under alkaline heating into volatile dimethylamine (DMA), which was selectively transferred through a hydrophobic PTFE membrane and trapped in an acidic acceptor solution, followed by pre-column derivatization with dansyl chloride to enable fluorescence detection. Mechanistic investigations confirmed DMA formation and identified additional alkaline degradation products (guanylurea-type intermediate, urea and guanidine) by HILIC and High-Resolution Time-of-Flight Mass Spectrometry, providing the chemical basis for the indirect workflow. Computational fluid dynamics simulations indicated focused headspace flow across the membrane (57.6% of total flow), negligible trans-membrane pressure (<0.5 Pa) and a moderated membrane temperature (∼49°C) under an 80°C heat source, rationalizing efficient transfer and reduced secondary volatilization. Key parameters were optimized, including heating time, absorption configuration, derivatization conditions. Under optimized conditions, the method was linear over 20-100 μg/mL (R=0.9924) with a limit of detectionof 0.002 μg/mL (S/N=3). Applicability was demonstrated in corn silk tea and sour jujube kernel tea, giving recoveries of 89.2-99.3% at 100 μg/mL and 95.4–102.0% across spiking levels, with no evident chromatographic interferences. The Alkaline Hydrolysis-Array Gas Membrane Separation-HPLC-FL approach integrates conversion, membrane-based separation and fluorescence derivatization, offering an efficient and solvent-minimized option for routine screening of metformin adulteration in complex matrices.
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高影响因子
CHROMATOGRAPHIA
·
2022
·Vol. 86
·期 1
·55-62
·
IF 2.213
Zhang Caiyu,Li Wei,Ning Baoming
This study aimed to develop and validate a high-performance liquid chromatography system combined with a single-quadrupole Dalton mass detector for the separation and determination of pidotimod (( R )-3-[( S )-(5-oxo-2-pyrrolidinyl)carbonyl]-thiazolidine-4-carboxylic acid) and its three isomers. The separations were achieved using a Lux Amylose-1 column operated at 40 °C using acetonitrile/0.1% trifluoroacetate (TFA) and isopropanol/0.1% TFA (90:10, v / v ). The enantiorecognition mechanism was also elucidated using the ORCA 5 program. Four isomers were successfully separated with a resolution (Rs) > 1.5, with the method showing satisfactory linearity in the ranges of 0.2 to 3.5 μg·mL −1 ( S,R; S,S ) and 0.5 to 3.5 μg·mL −1 ( R,S; R,R ), along with good specificity, accuracy, and precision. Further, three batches of pidotimod oral solutions were evaluated and the S,S -isomer in each batch was detected at about 0.05%. Moreover, computational evaluations suggested that the sorbent-analyte interactions of amylose tris(3,5-dimethylphenycarbamate) can be used to successfully interpret and even predict the chromatographic separation results. The validated method showed high sensitivity and can potentially be used to analyze the isomer impurities of raw materials for quality control purposes.
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Drug Research
·
2023
·Vol. 73
·期 06
·335-340
·
IF 2.2
Guo Haihua,Zhang Rui,Deng Liangjun,Li Meng,Li Sha,Zhao Suqing
Background Inhalation preparation involves liquid or solid raw materials for delivering to lungs as aerosol or vapor. The liquid preparation for nebulizer is effective for convenient use and patient compliance and it has been extensively used in the treatment of clinical lung diseases. Clinical staff often mixes the compound ipratropium bromide with beclomethasone propionate and budesonide inhaler but reference values of inhalants for clinical use need to be established for simplifying the operation procedure. The high-performance liquid chromatography (HPLC) method of compound ipratropium bromide solution, beclomethasone propionate suspension and budesonide suspension after mixed atomization was studied. Methods The specificity, linearity, recovery (accuracy), precision and stability of compound ipratropium bromide, beclomethasone propionate and budesonide were tested to verify the developed liquid phase method. Results The developed liquid phase method had high specificity, linear R2≥0,999, recovery (accuracy) RSD (relative standard deviation) less than 2%, precision RSD less than 2,0%, and stability RSD less than 2,0%. Conclusion The liquid phase methodology developed in this study can be used for the determination of compound ipratropium bromide mixed with beclomethasone propionate and budesonide. The current methodology can also be used to provide a reference for the determination of its content after mixing, and further data support for its clinical medication.
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高影响因子
MICROCHIMICA ACTA
·
2022
·Vol. 189
·期 12
·1-10
·
IF 6.408
Sun Min,Wang Xiuqin,Ding Yali,Feng Juanjuan
In order to improve the selectivity and stability of melamine–formaldehyde (MF) aerogel, it was composited with TiO 2 aerogel. A TiO 2 -MF hybrid aerogel was in situ prepared on the surface of carbon fibers for in-tube solid-phase microextraction (SPME). The extraction performance of TiO 2 -MF aerogel was regulated by changing the ratio of TiO 2 sol and MF sol during the material preparation. Coupled with high-performance liquid chromatography-diode array detection (HPLC–DAD), the extraction tube filled by TiO 2 -MF aerogel-coated carbon fibers was evaluated with several types of environmental pollutants including polycyclic aromatic hydrocarbons (PAHs), estrogens, and ultraviolet filters. Because of favourable extraction performance of PAHs they were selected as model analytes, and some important influence factors were optimized for satisfactory sensitivity. The detection limits were in the range 0.05–0.10 μg L −1 , owing to high enrichment factors (653–1007). The online in-tube SPME-HPLC–DAD method was verified for the determination of trace PAHs in environmental water samples, and acceptable recovery (70–118%) was achieved. The analytical methods also displayed some advantages in comparison with other reports. Moreover, the extraction tube exhibited satisfactory chemical stability. Graphical abstract
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JOURNAL OF CHROMATOGRAPHY A
·
2022
·
IF 4.601
Haokun Zhang,Youfang Huang,Xiaochong Song,Jinghe Peng,Yiqi Xu,Yu Zhang,Xiaojia Huang
Efficient extraction is a vital step in mercury speciation. In this context, using 4-vinylbenzeneboronic acid and 9-vinylanthracene as functional monomers, a new magnetic adsorbent was fabricated according to one-pot hydrothermal approach. Various characterization results prove the as-prepared adsorbent presented abundant functional groups and saturation magnetism. Combining with magnetic solid phase extraction (MSPE), the adsorbent exhibited satisfactory entrapment performance towards different mercury species which had been pre-coordinated with dithizone to form metal-organic coordination. A series of parameters influencing the extraction performance were inspected in detail. Under the most beneficial conditions, sensitive and reliable approach to quantify trace methylmercury, ethylmercury, phenylmercury and inorganic mercury in aqueous samples was developed by the combination of HPLC/DAD. Limits of detection and precision located in the ranges of 0.012–0.074 µg/L and 2.5–9.8%, respectively. Recoveries with low, medium and high fortified contents in actual waters varied from 79.8 to 119%. Confirmatory experiments were performed to evidence the accuracy and reliability of established approach. In addition, a possible mechanism was suggested based on the chemical nature of analytes, extraction conditions and characterization results.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2022
·
IF 3.571
Mengmeng Song,Xianjie Sheng,Genyi Ye,Zhuicheng Xu,Xinru Li,Tong Xie,Haishan Deng,An Kang
Gut microbiota-derived tryptophan (TRP) metabolites, especially the indole derivatives, function as critical modulators of intestinal immune function and integrity via modulating the aryl hydrocarbon receptor pathway. Selective enrichment of these indole metabolites in biological samples is important for quantitative determination by routine methods such as HPLC. Here, we report a molecularly imprinted polymer (MIP) for solid-phase extraction (SPE) of TRP-derived indole metabolites from faeces of mice. The MIP was synthesized by surface polymerization by using indole-3-acetic acid (IAA) and acrylamide after cross-linking by ethylene glycol dimethacrylate (EGDMA) and initialed by 2′,2-azobisisobutyronitrile (AIBN). The MIPs were then characterized by transmission electron microscope (TEM) and fourier transform infrared spectroscopy (FTIR), and the adsorption capacity, selectivity and reusability of MIPs were systematically evaluated. Results showed that IAA-MIPs showed a uniformly distributed nanoshell layer with a thin shell thickness of 26 nm . The IAA-MIPs could selectively adsorb IAA, indole-3-propionic acid (IPA), and indole-3-lactic acid (ILA) in a mixed solution that also contains TRP and tyrosine. The adsorption capacity of IAA-MIPs only slightly decreased with the increase of recycling use. As purification material for SPE, the IAA-imprinted polymers (IAA-MIPs) were successfully applied to extract IAA, IPA, and ILA from normal and colitis mice for HPLC determination. Collectively, these surface molecularly imprinted polymers could find extensive use to selective enrichment of microbiota-derived indole metabolites in biological samples.
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高影响因子
JOURNAL OF PHARMACY AND PHARMACOLOGY
·
2022
·Vol. 74
·期 7
·1040-1050
·
IF 4.81
Zhang Sijie,Gong Xingchu,Qu Haibin
ObjectivesTo investigate the feasibility of using near-infrared spectroscopy for rapid determination of main organic acids in Ginkgo biloba leaf extract (EGBL).MethodsMain organic acids in EGBL were assayed using the HPLC method. Critical factors of the chromatographic separation were optimized by a novel analytical quality by design approach. Partial least squares-discriminant analysis (PLS-DA) was performed to screen the marker components, and principal component analysis (PCA) was utilized to distinguish the different samples. Then, spectral quantification potential was investigated using PLS and support vector machine (SVM) approaches. For modelling, different spectral preprocessing and wavelength selection methods were systematically compared.Key findingsIt was found that quinic acid, protocatechuic acid and 6-hydroxykynurenic acid were identified as possible index components. PLS-DA based on contents and PCA based on near-infrared spectra can both effectively distinguish the different EGBL samples. The calibration models with wonderful prediction performance can be both developed by the PLS and SVM algorithms.ConclusionsNIR spectroscopy combined with chemometrics can realize the rapid and non-destructive qualitative and quantitative analysis of EGBL. The proposed method may be applied to quality control of EGBL and other natural products in commercial use.
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FOOD CHEMISTRY
·
2022
·
IF 9.231
Yi Zhang,Zhi-Liang Yuan,Xin-Yu Deng,Hao-Dong Wei,Wen-Long Wang,Zhenghua Xu,Yongwei Feng,Xueli Shi
The residues of bisphenol A (BPA) in milk packaging may transfer to milk, adversely affecting the human endocrine system. Consequently, to analyse or monitor BPA, it is imperative to develop rapid and effective approaches to BPA extraction from milk and milk packing as BPA is usually present in trace levels. Herein, we developed a rapid, simple, and low-cost dispersive-membrane-solid-phase-extraction (DME) for BPA with MIL-101(Cr) mixed-matrix-membrane (MMM). The MMM had large surface area (1322.09 m 2 /g) and pore volume (0.65 cm 3 /g), possessed great extraction efficiency of BPA, and kept more than 90% extraction efficiency after 20 times of reuse. Using the developed MIL-101(Cr)-MMM-based DME coupled with HPLC-fluorescence detector, we received an adequate linearity in the range of 0.1 ∼ 50 μg/L BPA and a limit of detection as low as 16 ng/L under optimized conditions. The recoveries of BPA in milk and milk bottles were from 74.2% to 110.6%, with RSDs less than 9.4%.
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ANALYTICAL LETTERS
·
2022
·
IF 2.267
Yu Huang,Yi Wu,Wenhui Li,Xiaohui Yan,Dapeng Wu
Highly spherical porous silica particles (PSPs) with a controlled pore size were prepared by ultrasonic spray drying and were used as a packing material for high-performance liquid chromatography (HPLC). By using organic additives added to the silica sol as porogens instead of low-melting salts, choosing the size of the colloidal SiO2 particles, and varying the type and the ratio of additives, the pore size of the PSPs was finely tuned from 2.9 to 34.4 nm. Subsequently, PSPs having pore sizes of 7.4, 13.5, and 29.0 nm were modified by chlorodimethyloctadecylsilane (PSPs-C18), and HPLC columns packed with the different PSPs-C18 were evaluated systematically using aromatic compounds and alkylbenzene derivatives as probes. A plate number of 81,000/m and the relative standard deviation of less than 1% in the retention time were obtained for pentylbenzene over 100 injection and HPLC separation cycles for the 7.4-PSPs-C18 column. Five proteins were also separated within 25 min using the 29.0-PSPs-C18 column.
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高影响因子
FOOD CHEMISTRY
·
2022
·
IF 9.231
Dan Wei,Ao Pan,Can Zhang,Ming Guo,Chaoyan Lou,Ju Zhang,Huizhen Wu,Xu Wang
A simple, rapid and sensitive vortex-assisted magnetic solid phase extraction (MSPE) method using core–shell structured magnetic covalent organic frameworks (Fe 3 O 4 /COF-TpBD) as adsorbents was established for simultaneous determination of aflatoxins, ochratoxins and enniatins in maize before high-performance chromatography tandem spectrometry detection. Fe 3 O 4 /COF-TpBD was facilely fabricated, characterized, and applied for simultaneous extraction of ten mycotoxins from maize. Key parameters affecting MSPE efficiency were investigated. The method possessed good linearity (0.05–50 μg/kg), high sensitivity (0.02–1.67 µg/kg for limits of detection), and satisfactory recoveries (73.8–105.3 %), with relative standard deviations less than 8.5 %. The amount of adsorbent used (5 mg) and the time required (0.5 min each for adsorption and for desorption) for MSPE were greatly shortened in comparison with the previous reports. Therefore, the fabricated Fe 3 O 4 /COF-TpBD exhibited a great potential for rapid extraction of common mycotoxins in maize, which can be attributed to its multiple interactions with the target mycotoxins.
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高影响因子
Foods
·
2022
·Vol. 11
·期 13
·1843
·
IF 5.561
Lanlan Wei,Yanan Chen,Dongliang Shao,Jingjun Li
In this study, a packed-fiber solid-phase extraction (PFSPE)-based method was developed to simultaneously detect nine quinolones, including enrofloxacin (ENR), ciprofloxacin (CIP), ofloxacin (OFL), pefloxacin (PEF), lomefloxacin (LOM), norfloxacin (NOR), sarafloxacin (SAR), danofloxacin (DAN), and difloxacin (DIF), in pure milk, using high-performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS). Polystyrene (PS) and polyacrylonitrile (PAN) were combined to form PS-PAN composite nanofibers through electrospinning. The nanofibers were used to prepare the home-made extraction columns, and the process was optimized and validated using blank pure milk. The analytical method showed high accuracy, and the recoveries were 88.68–97.63%. Intra-day and inter-day relative standard deviations were in the ranges of 1.11–6.77% and 2.26–7.17%, respectively. In addition, the developed method showed good linearity (R2≥ 0.995) and low method quantification limits for the nine quinolones (between 1.0–100 ng/mL) for all samples studied. The nine quinolones in the complex matrix were directly extracted using 4.0 mg of PS-PAN composite nanofibers as a sorbent and completely eluted in 100 μL elution solvent. Therefore, the developed PFSPE-HPLC-MS/MS is a sensitive and cost-effective technique that can effectively detect and control nine quinolones in dairy products.Keywords:polystyrene-polyacrylonitrile nanofibers;quinolones;packed-fiber solid-phase extraction;HPLC-MS/MS;pure liquid milk
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高影响因子
CHROMATOGRAPHIA
·
2021
·Vol. 84
·期 11
·1057-1064
·
IF 2.044
Zhang Hanzhi,Li Feng,Dun Junling,Sun Ning,Liu Hao,Chen Guiliang
An analysis strategy that can simultaneously determine the amino acid site information and configuration for polymyxin (PM) components is reported in this study. The main components of PMB1, PMB2, and PMB1-I (the Leucine at position 7 changed to be Isoleucine) were purified from the mixture of PMB. The PMB component was hydrolyzed by hydrochloric acid to be a mixture of amino acids, which were derivatized with Marfey’s reagent of N α -(5-fluoro-2,4-dinitrophenyl)- l -alanine amide ( l -FDAA), and then, the configurations of amino acids were easily determined by HPLC–MS. However, the aforementioned method could not offer the information of amino acid at each site, a specific enzymatic hydrolysis method combined Edman degradation was developed. The fatty acyl-diaminobutyric acid (position 1) of PMB component was removed by ficin, and the PMB components were transformed to be PMB nonapeptide. The amino acids at each site of the nonapeptide were determined by N-terminal sequencing. Combining the results of the above methods, the amino acid information and configuration of each site in PM components can be determined, especially the l -Leucine and l -Isoleucine in PMB1 and PMB1-I. The workflow was useful for other PM analogues to identify the sequence and configuration for quality control.
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危险品化学品经营许可证（带存储）