JOURNAL OF CHROMATOGRAPHY A
·
2025
·
IF 4
Liang Qi,Xinting Zhang,Longjiang Li,Xilan Li,Xiangna Chang
Prolonged use of cosmetics containing banned fluoroquinolones can cause skin disorders and increase drug resistance. The QuEChERS method holds considerable application prospect in the pretreatment of cosmetic samples. Although octadecyl (C 18 )-bonded silica sorbent is commonly used as a QuEChERS clean-up material, the conventionally commercially available bulk C 18 sorbent is relatively costly and has a limited purification mechanism. In this study, using dendritic silica sphere (dSiO 2 ) as the substrate, and through the condensation reaction between cyanuric chloride (CNCl) and the amino group, a dNSiO 2 -CNCl-C 18 sorbent was synthesized. The sorbent was characterized using infrared spectroscopy, transmission electron microscopy, surface area and pore size analysis, and water contact angle measurements. The experimental results regarding the matrix removal from the model cosmetic lotion showed that dNSiO 2 -CNCl-C 18 exhibited a higher matrix removal efficiency compared to a commercial C 18 sorbent. Furthermore, a QuEChERS-HPLC-FLD method was developed using dNSiO 2 -CNCl-C 18 for the simultaneous detection of four fluoroquinolones, norfloxacin (NOR), pefloxacin (PEF), enrofloxacin (ENR), and difloxacin (DIF). The linear ranges were 0.10 to 100.0 μg L −1 for NOR and PEF, and 0.05 to 100.0 μg L −1 for ENR and DIF, with coefficient of determination exceeding 0.999. Satisfactory spiked recoveries for the lotion sample ranged from 91.5% to 107.0%, with intra-day and inter-day precision values not exceeding 7.6%. The established method was subsequently validated through its successful application in additional cream and emulsion samples. dNSiO 2 -CNCl-C 18 exhibits low synthesis costs and demonstrates promising potential for matrix purification in various complex samples, facilitating the rapid determination of target compounds.
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FOOD CHEMISTRY
·
2025
·
IF 9.8
Ying Li,Yu Zhang,Li Zhang,Jun Dang
The screening of enzyme inhibitors faces challenges such as low efficiency. In this study, a novel online HPLC-FLD/pancreatic lipase recognition system was developed for the first time. The optimal operating parameters were established as a flow rate of 1 mL/min, with excitation and emission wavelengths for pancreatic lipase set at 221 nm and 303 nm, respectively. The effectiveness of this system was validated using orlistat. Subsequently, this system was applied to Lycium ruthenicum , where two petunidin-based anthocyanins pancreatic lipase inhibitors were efficiently isolated using medium-pressure liquid chromatography. Molecular docking elucidated that compounds 1 and 2 interact with the serine residue of pancreatic lipase, exhibiting binding energies of −13.12 kcal/mol and −12.22 kcal/mol, respectively. Enzymatic assays showed that the half-maximal inhibitory concentrations of compounds 1 and 2 were 9.67 μM and 147.37 μM, respectively. These docking and inhibition results confirm the system for efficiently discovering pancreatic lipase inhibitors.
研究领域:
植物化学
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分析化学
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酶学
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天然产物化学
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药物发现
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Food Additives and Contaminants Part A-Chemistry Analysis Control Exposure & Risk Assessment
·
2021
·
IF 3.057
Shaomin Ma,Xiuyi Jin,Huan Wei,Yue Liu,Ming Guo
In this paper, novel high extraction efficiency hydrophobic eutectic solvents (DESs), n-octanoic acid as a hydrogen bond donor (HBD) and menthol as a hydrogen bond acceptor (HBA), were selected from five hydrophobic DESs to extract trace diphenylamine (DPA) in fruits apple, pear and orange under ultrasonic-assisted liquid-liquid micro-extraction (UA-LLME) technology before high-performance liquid chromatography (HPLC) analysis. Working parameters such as the DESs type, molar ratio, extractant volume, and ultrasonic time of the LLME hydrophobic DESs technology were optimised. Average recoveries between 96% and 108% were obtained on actual samples. This method gave lower detection limit (LOD) than other existing methods due to combining the high-efficiency extraction of hydrophobic DES and high sensitivity of fluorescence detector. This method was sensitive and eco-friendly, and can be used for the determination of trace components in fruits.
研究领域:
分析化学
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食品科学
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FOOD CHEMISTRY
·
2020
·
IF 6.306
Shuying Han,Yilin Song,Jiachun Hu,Rui Liu,Yumei Chi,An Kang,Haishan Deng,Dong Zhu
An on-line enrichment-liquid chromatography-fluorescence detection (LC-FD) method was developed for simultaneous determination of nine bisphenols (BPs). In this process, we predicted the separation based on an in-house developed software allowing for calculating both retention time ( t R ) and half-peak width ( W 1/2 ) of the solute by mobile phase fraction ( φ ) under gradient conditions. The proposed strategy was applied to separation prediction of BPs with high accuracy. Under the optimized conditions, good linearity was obtained with the correlation coefficients ( R 2 ) ranging from 0.998 to 1.000. The recoveries in spiked samples were 91.3–110.7% with the intra-day and inter-day relative standard deviation ranging 0.4–9.6% and 0.5–10.2%, respectively. The limits of detection and quantification were 0.13–66.7 ng L −1 and 0.40–200 ng L −1 . The developed approach was used to monitor the nine BPs in 28 children’s water bottles. The developed method provides an effective way for monitoring bisphenols in other similar matrix.
研究领域:
分析化学
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环境科学
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毒理学
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高影响因子
MICROCHIMICA ACTA
·
2020
·Vol. 187
·期 4
·1-8
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IF 6.232
Li Lin,Han Dandan,Wang Mingwei,Han Yehong,Yan Hongyuan
A composite was synthesized from two-dimensional molybdenum disulfide (MoS 2 ) nanosheets and hypercrosslinked polymers (HCP), and the composite was characterized by infrared spectroscopy, scanning electron microscopy, and specific surface area. The fluffy and porous structure and multiple adsorption sites (π-interaction, static electricity, hydrogen bonding) make it ideal for use as an adsorbent. A pipette tip solid-phase extraction with the composite as the adsorbent combined with HPLC–FLD was developed to determine trace amounts of polycyclic aromatic hydrocarbons (phenanthrene, anthracene, fluoranthene, pyrene, benzo(α)anthracene) in environmental water. Under optimal extraction conditions, the method has a wide linear range (0.5–100 ng mL −1 ) and low limit of detection (0.024–0.099 ng mL −1 ), and the recoveries of PAHs from spiked environmental water were 73.8% to 123.6% (relative standard deviation ≤ 6.7%, n = 3).
Schematic representation of a three-dimensional molybdenum disulfide–ethylenediamine–hypercrosslinked polymer composite (MoS 2 –EDA–HCP) using pipette tip solid-phase extraction adsorbent for extracting trace levels of polycyclic aromatic hydrocarbons (PAHs) prior to HPLC–FLD. HCP, hypercrosslinked polymer; MoS 2 , molybdenum disulfide; EDA, ethylenediamine
研究领域:
环境科学
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分析化学
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BIOMEDICAL CHROMATOGRAPHY
·
2018
·Vol. 32
·期 11
·e4338
·
IF 1.688
Dan Huang,Qing-Song Jiang,Jun-Qing Yang,Ting Cui,Nian-Ru Wang,Ting-Ting Du,Xin-Hui Jiang
The determination of amino acids and monoamine with actions like neurotransmitters or modulators has become increasingly important for studying the relationship between the dysfunction of neurotransmitters and the pathogenesis of diabetic encephalopathy. Here, a high-performance liquid chromatography with fluorescence detection method was developed to simultaneously determine nine monoamines and amino acids including three excitatory neurotransmitters (aspartate, glutamate, and serotonin), four inhibitory neurotransmitters (glycine, γ -aminobutyric acid, taurine, dopamine), a precursor of 5-HT (tryptophan) and methionine using homoserine as the internal standard. The separation was performed on a BDS column with methanol-buffer solution of 35 mmol/L sodium acetate and 5 mmol/L citric acid (pH 6.0) using a simple gradient elution. Several parameters including specificity, precision, and recovery were validated after optimization of the analytical conditions. The developed method was successfully applied to determine the cortex and the hippocampus samples from Sprague–Dawley rats. Our results showed that various neurotransmitters involved in diabetes mellitus may tend to be differentially modulated and present a different alteration tendency at different time course, which might be associated with the duration of diabetes mellitus.
研究领域:
神经科学
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药理学
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分析化学
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糖尿病研究
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2013
·
IF 2.487
Jian-Yao Wang,Hai-Long Wu,Yan-Mei Sun,Hui-Wen Gu,Zhi Liu,Ya-Juan Liu,Ru-Qin Yu
A novel strategy that combines the chemometrics method with high performance liquid chromatography with fluorescence detector (HPLC–FLD) was developed for the simultaneous determination of seven phenolic antioxidants in six kinds of oil samples. After a simple dilution step, oil samples can be directly injected into the detecting system and the data were measured in a short time with a chromatographic system operating in the gradient elution mode. Since the chromatographic and spectral peaks among interesting analytes and interferences were heavily overlapped, second-order calibration method based on alternating trilinear decomposition (ATLD) algorithm which fully exploiting the second-order advantage was adopted. Successful resolution was obtained in the presence of different matrix interferences in different oil samples, and the developed approach allows the quantification of the antioxidants at levels found in edible vegetable oils, without the necessity of applying either preconcentration or extraction steps, moreover, a column washing is also not required. Meanwhile, the effectiveness and reproducibility of the proposed method were also validated by some statistical parameters like root mean squared error of prediction (RMSEP), limits of detection (LOD) and relative standard deviation (RSD). Then the proposed method was compared with several commonly selected methods in sample preparation, elution time and LOD.
研究领域:
分析化学
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食品科学
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TALANTA
·
2013
·
IF 3.498
Di Pan,Jianping Wang,Chunyan Chen,Chen'an Huang,Qingyun Cai,Shouzhuo Yao
In this work, ultrasonic assisted extraction combined with solid phase extraction (SPE) was applied in the analysis of polycyclic aromatic hydrocarbons (PAHs) in environment samples. A titania nanotubes/titanium plate was modified with n-octadecanethiol monolayer-protected Ag nanoparticles , and developed as the adsorbent in SPE of PAHs. Six different PAHs in soil samples were analyzed with high performance liquid chromatography-fluorescence detection. The experiment conditions including the deposition time of Ag nanoparticles, extraction solvent properties, the amount of extraction solvent, the amount of organic modifier, extraction time, and desorption solvent properties were optimized. Under the optimized conditions, good linearity and low limits of detection of 0.0015–0.4 ng g −1 were obtained. The analysis of PAHs in real soil samples gave satisfactory recoveries ranging from 70.32% to 115.51% with 3.14%–13.56% intra-day relative standard deviations (RSD) and 4.92%–14.87% inter-day RSD.
研究领域:
环境科学
·
分析化学
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BIOMEDICAL CHROMATOGRAPHY
·
2019
·Vol. 34
·期 3
·e4767
·
IF 1.748
Yong-hong Liu,Ting-ting Du,Jing-yuan Wan,Hua Zhao,Dan Huang,Jian-sha Li,Xin-hui Jiang
Disorders of certain branched-chain amino acids may be associated with the occurrence and development of non-alcoholic fatty liver disease. Measurement of related branched-chain amino acid levels could provide a reference for the clinical and scientific research of the non-alcoholic fatty liver disease. An established HPLC–FLD method was used to quantify aspartic acid, glutamate, glutamine, glycine, taurine, tyrosine, 4-amino butanoic acid, tryptophan, methionine, valine, phenylalanine, isoleucine and leucine in mouse brain tissue. Brain tissue samples mixed with internal standard (3-aminobutyric acid) were processed, then derivatized with 2- O -phthaldialdehyde, and finally separated on an ODS2 column through gradient elution at a flow rate of 1.0 ml·min −1 . The excitation and emission wavelengths were set at 340 and 455 nm, respectively. The mobile phase A was 100% methanol and the mobile phase B consisted of 30 mmol·L −1 sodium acetate (pH 6.8). The injection volume was 20 μl and the single run time was 45 min. Several parameters, accuracy, precision, and stability, were verified and the results showed the established method had good sensitivity and resolution for all of the 13 compounds and internal standard in mouse brain.
研究领域:
生物化学
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医学研究
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分析化学
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JOURNAL OF CHROMATOGRAPHY A
·
2025
·
IF 4
Wen Hou,Ya-Qi Zhu,Yue-Jiao Yang,Qiong-Wei Yu
Loofah sponges (LS) were simply treated by alkaline solution and then used as solid-phase extraction (SPE) adsorbent to extract bisphenols from environmental water samples for the first time. As naturally material, LS exhibited an excellent adsorption performance for bisphenol compounds due to their particular functional groups such as hydroxyl, carboxyl, amino, and other active groups. Key extraction conditions were optimized, including adsorbent amount, washing solvent volume, sample pH, ionic strength, sample loading flow rate, eluent type, and elution solvent volume. Under the optimal extraction conditions (200 mg adsorbent amount and 5.0 mL eluent volume), a method was developed for analyzing five bisphenols in environmental waters by combining LS-based SPE with high-performance liquid chromatography-fluorescence detection (HPLC-FLD). This analytical method showed excellent linearity within BP concentration range of 0.5-500 ng/mL and low detection limits (0.077-0.225 ng/mL). The recoveries of five bisphenols ranged from 78.6 % to 112 % with inter-day and inter-day precision less than 5.1 %. This method was successfully applied to the analysis of bisphenols in water samples with various water sources including river, lake, tap water, bottled water, and barrelled water. The proposed analytical method is low-cost, efficient, and sensitive, offering an alternative strategy for monitoring bisphenols in enviromental water.
研究领域:
环境科学
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分析化学
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JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES
·
2021
·
IF 1.312
Yan Du,Jinhua Hu,Zhixiong Hu,Weinong Zhang,Yutang Qi,Yanpeng Zhang,Xiaomin Li,Yi Liu
In this paper, a sensitive method for the determination of 3-chloro-1,2-propanediol (3-MCPD) by high performance liquid chromatography-fluorescence detection (HPLC-FLD) was established, in which 9-(2-Hydroxypropyl) adenine (HP-Ade) was selected as the fluorescent derivatization reagent because of its good water solubility and hydrophobicity. The principle of the method lies in the origination of chloroacetaldehyde with the periodate oxidation of 3-MCPD and its' fluorescence derivatization by HP-Ade to produce a strong fluorescent substance, name as 1-N6-vinylidene-9-(2-hydroxypropyl)adenine (ε-HP-Ade), used for quantitative determination of 3-MCPD by HPLC-FLD. Some mobile phase conditions and incubation parameters related with the method features were studied and optimized. Under the optimal conditions, the method shows high sensitivity, good linearity (r2 = 0.999) and good repeatability (RSD% between 1.04% and 2.55%), the detection limit (LOD) and quantification limit (LOQ) were 0.02 ng/mL and 0.06 ng/mL respectively. It has been successfully applied for the determination of various edible vegetable oil samples, the chromatogram shows symmetrical peak shape, perfect separation and very “clean” profiles. In comparison with gas chromatography-mass spectrum (GC-MS), the pretreatment process of the proposed method was totally operated in aqueous phase, the instrument requirements and cost are relatively lower, thus it will provide another choice for the routine analysis of 3-MCPD.
研究领域:
分析化学
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食品科学
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JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
·
2013
·
IF 2.906
Zhixiong Hu,Peng Cheng,Mingli Guo,Weinong Zhang,Yutang Qi
A novel approach of periodate oxidation coupled with high-performance liquid chromatography (HPLC)–fluorescence detection (FLD) for the quantitative determination of 3-chloro-1,2-propanediol (3-MCPD) has been established. The essence of this approach lies in the production of chloroacetaldehyde by the oxidization cleavage of 3-MCPD with sodium periodate and the HPLC analysis of chloroacetaldehyde monitored by an FLD detector after fluorescence derivatization with adenine. The experimental parameters relating to the efficiency of the derivative reaction such as concentration of adenine, chloroacetaldehyde reaction temperature, and time were studied. Under the optimized conditions, the proposed method can provide high sensitivity, good linearity (r2 = 0.999), and repeatability (percent relative standard deviations between 2.57% and 3.44%), the limits of detection and quantification were 0.36 and 1.20 ng/mL, respectively, and the recoveries obtained for water samples were in the range 93.39–97.39%. This method has been successfully applied to the analysis of real water samples. Also this method has been successfully used for the analysis of vegetable oil samples after pretreatment with liquid–liquid extraction; the recoveries obtained by a spiking experiment with soybean oil ranged from 96.27% to 102.42%. In comparison with gas chromatography or gas chromatography–mass spectrometry, the proposed method can provide the advantages of simple instrumental requirement, easy operation, low cost, and high efficiency, thus making this approach another good choice for the sensitive determination of 3-MCPD.
研究领域:
食品科学
·
分析化学
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危险品化学品经营许可证（带存储）