JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2026
·
IF 2.5
Chuang Liu,Jianbin Ma,Qin Zhao,Yurong Du,Jun Dang
HPLC-FLD enabled recognition and tracking of PL-affinity peaks during separation. • PL-affinity peaks remained traceable across reversed-phase and HILIC separations. • Three compounds from S. tangutica , including 1 activator and 2 inhibitors. Background Translating biological recognition into chromatographic information that can continuously guide targeted isolation remains challenging in natural products. Methods HPLC coupled with fluorescence detection (HPLC–FLD) was combined with multimodal preparative chromatography to recognize, track, and isolate candidate pancreatic lipase (PL)-affinity ligands from Saxifraga tangutica . Their effects on PL were evaluated by activity and kinetic assays, with DFT calculations and molecular docking as complementary analyses. Results Three flavonoid glycosides with chromatographic purities above 95% were isolated: Q3XG (160.8 mg), Q3AG (167.9 mg), and Q3GG (623.1 mg). Q3XG activated PL with an EC₅₀ of 4.78 ± 0.95 μg/mL, whereas Q3AG and Q3GG inhibited PL with IC₅₀ values of 38.33 ± 1.97 and 43.86 ± 2.87 μg/mL, respectively. Kinetic analysis showed that Q3XG decreased the apparent K m and slightly increased the apparent V max, whereas Q3AG and Q3GG showed the opposite changes, consistent with mixed-type inhibition. DFT and docking analyses indicated differences in electronic properties and predicted PL-ligand interaction patterns. Conclusion Integration of HPLC–FLD with multimodal chromatography preserved the link between affinity signals and target peaks throughout chromatographic tracking, selectivity optimization, and preparative isolation, providing a practical route to functionally validated ligands from complex natural products. Download: Download high-res image (162KB) Download: Download full-size image
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高影响因子
Journal of Food Measurement and Characterization
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2026
·
IF 3.6
Guan Xiuping,Guo Xinbo
Folate are essential B-group vitamins involved in one-carbon metabolism and human health. Accurate determination of individual folate vitamers together with selected biosynthetic precursors remains analytically challenging because of their structural diversity, low endogenous concentrations, and distinct physicochemical properties. A sensitive and practical HPLC–FLD method was developed for the determination of individual folate vitamers together with selected biosynthetic precursors, and subsequently applied to selected plant-derived foods. The target analytes included dihydrofolate (DHF), tetrahydrofolate (THF), 5-methyltetrahydrofolate (5-MTHF), 5-formyltetrahydrofolate (5-FTHF), 10-formylfolic acid (10-FFA), folic acid (FA), p-aminobenzoic acid (p-ABA), and 7,8-dihydroneopterin (DHN). The method exhibited good linearity (R² > 0.994), satisfactory recoveries (73.01–100.80%), acceptable precision (RSD < 9%), and limits of detection reaching the “pmol” level for several analytes. The developed method was applied to selected plant-derived food samples, including cereals, soybeans, and vegetables, demonstrating its potential for characterizing differences in folate vitamer and precursor composition among the investigated food samples. Owing to its economical instrumentation, relatively simple sample pretreatment, and ability to quantify both folate vitamers and biosynthetic precursors, the proposed method provides a practical analytical tool for folate profiling in selected plant-derived foods, although further validation across additional food matrices would be required to establish broader applicability.
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高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
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2020
·Vol. 412
·期 19
·4725-4737
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IF 3.637
Fu Han,Xu Wu,Wang Haixiang,Liao Shenghua,Chen Guitang
This study was based on the specific binding ability of magnetic molecularly imprinted polymers (MMIPs) combined with a high-performance liquid chromatography-fluorescence detector (HPLC-FLD) for the rapid determination of zearalenone (ZEN) in cereals. A novel magnetic molecularly imprinted polymer was prepared by surface imprinting technology. Warfarin was used as a virtual template, 3-aminopropyl triethoxysilane (APTES) was used as the functional monomer, and tetraethyl orthosilicate (TEOS) was used as the cross-linking agent. Analysis by a vibrating sample magnetometer (VSM), Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) showed that MMIPs were prepared with a particle size about 450 nm, the imprinted molecular layer accounting for 10.7% of the total mass, and saturation magnetization of about 34.54 emu/g. The maximum adsorption capacity ( Q max ) of the thermodynamic and kinetic adsorption experiments were 13.90 mg/g and 8.71 mg/g, respectively. The Langmuir model showed that the binding sites were uniformly distributed on the surface of the MMIPs. The Scatchard analysis showed that MMIPs had two types of binding sites with Q max of 8.22 mg/g and 15.37 mg/g, respectively. In actual sample detection, the limit of detection (LOD) and limit of quantification (LOQ) were 0.4 ng/kg and 0.9 ng/kg, respectively. The sample recovery rate was 90.56–99.96%, the daytime stability was 1.35–2.87%. These results showed that MMIPs had good performance in selectively identifying ZEN and were suitable for determining ZEN in cereals.
研究领域:
食品科学
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分析化学
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
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2017
·Vol. 31
·期 8
·e3937
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IF 1.613
Ting Cui,Hong-Mei Qiu,Dan Huang,Qi-Xin Zhou,Xiao-Yan Fu,Hai-Yan Li,Xin-Hui Jiang
The determination of amino acids with actions like neurotransmitters or modulators has been increasingly important for diagnosis in many neuropsychiatric diseases. A rapid and simple high-performance liquid chromatography with fluorescence detection method was developed for simultaneous determination of seven amino acids: aspartate (Asp), glutamate (Glu), serine (Ser), glutamine (Gln), glycine (Gly), taurine (Tau) and γ-aminobutyric` acid (GABA). Homoserine was used as an internal standard. The analysis was performed on a BDS column with methanol and 50 m m sodium acetate solution (pH 6.5) using a simple gradient elution. Several parameters of the developed method were validated including linearity, accuracy, precision, extraction recovery and stability, which were within the acceptable range. The method was successfully applied to determination of real samples: hippocampus and cortex in depressed rats exposed to chronically unpredictable stress in order to study if there existed differences in the seven amino acids levels between depressed rats and control. The results showed that Asp, Gly, Tau and GABA significantly decreased with increasing Gln in the hippocampus of depressed rats, compared with that of the control group, among which obviously lower level of Asp and higher level of Gln in cortex were observed. The analytical method and the results could be useful for clinical diagnosis and further insight into pathophysiological mechanism of depression.
研究领域:
神经科学
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分析化学
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精神病学
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高影响因子
ECOTOXICOLOGY AND ENVIRONMENTAL SAFETY
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2021
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IF 6.291
Peipei Zhou,Rui Wang,Ru Fan,Xiaoran Yang,He Mei,Huaiyu Chen,Huili Wang,Zhenfeng Wang,Xuedong Wang
Herein, a kind of novel multi-layer core-shell nanocomposites (NSPN) was prepared by employing SiO 2 and polyvinylpyrrolidone (PVP) polymers as modifiers and amino-functionalized metal-organic frameworks (NH 2 -MIL101(Fe)) as coating. It was referred to as the NSPN and ILs-based effervescence-assisted dispersive solid-phase microextraction, hereafter abbreviated as NIE-DSM. In terms of extraction efficiency, SiO 2 and PVP as modifiers and NH 2 -MIL(Fe) as coating onto the surface of NiFe 2 O 4 cores played a synergistically enhancing effect on adsorption/extraction. Effervescent tablets were prepared by integrating the NSPN magnetic nanoparticles as adsorbents with imidazolium-based ionic liquids (ILs) as extractants as well as acidic and alkaline sources. Under vigorous dispersion of CO 2 bubbles, the NIE-DSM method realized the goal of rapidly diffusing and separating the adsorbent/extractant (~3 min) without needing conventional vortexing or centrifugation step. Consequently, the NIE-DSM approach combined dispersion and adsorption/extractant in a synchronous way. Under optimized conditions, the NIE-DSM/HPLC-FLD method gave low limits of detection (0.008–0.034 μg kg −1 ) and satisfactory extraction recoveries (74.1–101.6%) for five polycyclic aromatic hydrocarbons (PAHs; fluorene, anthracene, pyrene, chrysene and benzo(a)pyrene) in milk samples. The intra-day and inter-day precision, expressed as relative standard deviations, was < 5.9% and 6.5%, respectively, demonstrating a high precision. Owing to no requirement for electrical power, this method shows great potential for outdoor monitoring of trace-level PAHs in food matrices.
研究领域:
分析化学
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环境科学
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食品科学
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DOI
PubMed
高影响因子
Heliyon
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2022
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IF 3.776
Sheng Xu,Jianli Bi,Wenfang Jin,Baolei Fan,Chunqi Qian
A high-performance liquid chromatography-fluorescence detection (HPLC-FLD) method was established for the determination of seven monosaccharides in Polygonatum sibiricum and Polygonatum odoratum . The polysaccharides were de-esterified, extracted, hydrolyzed and derivatized with p-aminobenzoic acid (PABA) to obtain fluorescently labeled monosaccharide compounds, which were finally detected by HPLC-FLD. Inertsil ODS-3, C18 chromatographic column (250 mm × 4.6 mm, 5 μm) was used for chromatography. The excitation wavelength (E x ) was 313 nm, and the emission wavelength (E m ) was 358 nm. Ethyl acetate extraction reduced the peaks of chromatogram and improved the detection sensitivity than other agents. The established method had high sensitivity, strong specificity, good linear relationship and recovery efficiency. The results showed that the roots and fibrous roots of Polygonatum sibiricum and Polygonatum odoratum contained these seven monosaccharides, and the highest monosaccharide content was mannose. The method of PABA-HPLC-FLD for determination of monosaccharide content in Polygonatum sibiricum and Polygonatum odoratum was sensitive and accurate. The method established in this work provides a feasible analytical tool for the study of polysaccharides, and the findings on polysaccharides from Polygonatum sibiricum and Polygonatum odoratum can provide guidance for the natural medicine industry.
研究领域:
植物化学
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中药学
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高影响因子
Analytical Methods
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2016
·Vol. 8
·期 12
·2620-2627
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IF 1.915
Xiaoyun Zhang,Ying Chen,Lin Li,Hua Qiao,Rui Wang,Jingman Ni,Jieqiong You,Kaikai Ma,Chenchen Fan,Quan Fang
The objective of this research is to develop a sensitive bioanalytical method and investigate the pharmacokinetics of a new chimeric peptide (BN-9) in rats. According to the analysis criteria, a reversed phase high performance liquid chromatography method with fluorescence detection (HPLC-FLD) was established and employed in monitoring the compound in rat plasma using doxorubicin (DOX) as the internal standard (IS). Fluorescent BN-9 and IS were extracted from plasma using dehydrated alcohol. The mobile phase was composed of acetonitrile and potassium dihydrogen phosphate buffer containing 0.05% trifluoroacetic acid (TFA) (pH 7.4; 0.02 M) (30 : 70, v/v) at 0.7 mL min−1. Fluorescence detection was conducted at 490 nm (excitation wavelength) and 520 nm (emission wavelength). The lower limit of quantification (LLOQ) was 0.009 µg mL−1. The intra-batch and inter-batch precisions were less than 8.116%, and the accuracy was within 5.632%. Blood samples were collected after intravenous administration of fluorescent BN-9 at the doses of 5, 10, and 20 mg kg−1 to rats. The main pharmacokinetic parameters were obtained by non-compartmental and compartmental analysis with DAS 2.1.1 software. The t1/2α values were 9.584 ± 5.137, 8.548 ± 2.093 and 9.621 ± 0.3224 min. The results showed that the method was successfully applied to investigate the pharmacokinetic profiles of fluorescent BN-9 following intravenous administration to rats.
研究领域:
分析化学
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药理学
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生物化学
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DOI
高影响因子
MICROCHEMICAL JOURNAL
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2026
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IF 5.1
Shiyu Li,Li Zhang,Haihua Zhang,Fang Yang,Jun Dang
Hyperlipidemia is closely linked to abnormal dietary lipid absorption, and pancreatic lipase (PL) is a key target for inhibiting intestinal lipid hydrolysis. Thus, the efficient discovery of PL inhibitors is crucial for treating the disease. However, existing recognition techniques suffer from false positives and disconnection from subsequent separation, hindering the exploration of natural product active components. This study developed an online high-performance liquid chromatography-fluorescence detection (HPLC-FLD) recognition system. It enables real-time mixing of chromatographic eluents with PL solution, forming protein-ligand complexes that yield characteristic negative peaks due to their lower fluorescence, thus enabling rapid localization of PL-binding components at corresponding retention times. Validation with orlistat as a reference standard confirmed the system's high precision, stability, and specificity. When applied to the crude extract of Sinacalia tangutica , this system recognized 15 active chromatographic peaks in a single analysis. Combined with an activity-guided progressive separation strategy, 16 compounds were obtained and exhibited PL inhibitory activity in vitro enzymatic assays. The therapeutic potential of phlorizin, one of inhibitors identified by our recognition system, was evaluated in hyperlipidemic mice. High-dose phlorizin lowered serum total cholesterol (TC) by 46.3% and triglyceride (TG) by 66.3%, reduced pancreatic PL content by 52.4%, raised fecal TG by 65.7%, alleviated hepatic steatosis and oxidative stress, with efficacy near orlistat. This integrated strategy of online recognition with activity-guided separation provides an efficient solution for the discovery of natural PL inhibitors with therapeutic potential.
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高影响因子
JOURNAL OF CHROMATOGRAPHIC SCIENCE
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2022
·
IF 1.555
Zhang Jing,Yang Junqing,Luo Ying,Li Jiansha,Gong Tao,Huang Suqiong,Xiong Yan,Jiang Xinhui
Using 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate as a pre-column derivatization reagent, optimized derivatization and chromatography parameters, a simple high-performance liquid chromatography fluorescence detector (HPLC–FLD) method was developed and validated to determine 23 related amines in plasma and cortex of C57BL/6 mice with cerebral ischemia–reperfusion injury. The prepared samples were separated on a ZORBAX SB-C18 column (4.6 mm × 250 mm, 5 μm) with 60% acetonitrile (ACN) and 20 mM sodium acetate solution (pH adjusted to 5.0 by phosphoric acid). All analytes achieved good separation within 1.2 h at a flow rate of 1 mL/min. The limits of detection and limits of detection quantitation of the method were ranged from (0.1–9.2) to (0.3–30.6) ng/mL, respectively. The analytical method was apt for simultaneously determining 23 amino acids in plasma and cortex. Our results revealed that the relevant amino acids were significantly altered (P < 0.05) in C57BL/6 mice.
研究领域:
分析化学
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神经生物学
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医学
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DOI
PubMed
高影响因子
MOLECULES
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2023
·Vol. 28
·期 16
·6103
·
IF 4.6
Lanlan Wei,Yanan Chen,Dongliang Shao,Jingjun Li
In this work, a sensitive analytical method based on packed-nanofiber solid-phase extraction (PFSPE), after derivatization with trichloroacetic acid and high-performance liquid chromatography with a fluorescence detector (HPLC-FLD), has been established for the determination of aflatoxins (AFs) in milk. Polystyrene polymeric multi-walled carbon nanotube (PS-MWCNT/OH) composite nanofibers were fabricated by electrospinning and used to prepare homemade extraction columns. The extraction efficiency of the HPLC-FLD analysis method was sufficiently investigated and validated. After the implementation of optimal conditions, all of the analytes were separated efficiently and the components of the milk matrix did not disturb the determination. The obtained linear ranges of the calibration curves were 0.2–20 ng/mL for AFTB1 and AFTG2, 0.1–10 ng/mL for AFTB2, and 0.4–40 ng/mL for AFTG1. The recoveries ranged between 80.22% and 96.21%. The relative standard deviations (RSDs) for the intra-day and inter-day results ranged from 2.81–6.43% to 3.42–7.75%, respectively. Generally, 11 mg of sorbent and 200 μL of elution solvent were used to directly extract all of the AFs from the milk matrix. Reported herein is the first utilization of PS-MWCNT/OH-PFSPE HPLC-FLD to simultaneously analyze the occurrence of aflatoxins in milk.Keywords:aflatoxins;packed-nanofiber solid-phase extraction (PFSPE);sample preparation;polystyrene polymeric multi-walled carbon nanotube (PS-MWCNT/OH);milk
研究领域:
食品科学
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分析化学
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产品关联
DOI
PubMed
高影响因子
Food Analytical Methods
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2017
·Vol. 10
·期 12
·3856-3865
·
IF 2.038
Zhou Kai,Liu Yao,Li Wen-Qian,Liu Gong-Liang,Wei Na,Sun Yuan-Ming,Bai Wei-Dong,Xu Zhen-Lin
A high-performance liquid chromatography with fluorescence detection (HPLC-FLD) method for ethyl carbamate (EC) determination in Chinese soy sauce was developed and used to predict EC precursors, and extraction, derivatization, and chromatographic conditions were optimized systematically. Under optimal conditions, the limit of detection, linear range, and recoveries were 3.91 μg/L, 12.87–274.87 μg/L, and 81.5–95.4%, respectively. The method precision was less than 8.9% (RSD) and no significant difference was found between EC determinations measured by HPLC-FLD and GC/MS. Using the proposed HPLC-FLD method, the EC contents in Chinese soy sauces ranged from not detected to 64.88 μg/L ( n = 19). Except for one soy sauce brand, the EC contents in low-salt solid-state fermented (LSF) soy sauces were lower than those in high-salt liquid fermented (HLF) soy sauces and were mainly affected by alcohol content. Moreover, the free ornithine and total arginine contents were significantly correlated with EC content in the soy sauce products. The results of this work provide a foundation for further study of EC formation and inhibition in Chinese soy sauces.
研究领域:
食品科学
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分析化学
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DOI
高影响因子
FOOD CHEMISTRY
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2014
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IF 3.259
Ping Qi,Zhihao Lin,Jiaxu Li,ChengLong Wang,WeiWei Meng,Hong Hong,Xuewu Zhang
In this work, a simple, rapid and sensitive analytical method for the determination of rhodamine B in chili-containing foodstuffs is described. The dye is extracted from samples with methanol and analysed without further cleanup procedure by high-performance liquid chromatography (HPLC) coupled to fluorescence detection (FLD). The influence of matrix fluorescent compounds (capsaicin and dihydrocapsaicin) on the analysis was overcome by the optimisation of mobile-phase composition. The limit of determination (LOD) and limit of quantification (LOQ) were 3.7 and 10 μg/kg, respectively. Validation data show a good repeatability and within-lab reproducibility with relative standard deviations <10%. The overall recoveries are in the range of 98–103% in chili powder and in the range of 87–100% in chili oil depending on the concentration of rhodamine B in foodstuffs. This method is suitable for the routine analysis of rhodamine B due to its sensitivity, simplicity, reasonable time and cost.
研究领域:
食品科学
·
分析化学
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产品关联
DOI
PubMed
高影响因子
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