MOLECULES
·
2023
·Vol. 28
·期 14
·5309
·
IF 4.6
Shi-Hui Lu,Xiao-Na Liang,Xiao-Jin Nong,Ran Chen,Xiu-Xia Li
Trans-p-hydroxycinnamic acid and its esters in the leaves ofLigustrum robustummight be a new resource to prevent diabetes and its complications. In the present study, a new HPLC-UV method using hydrolyzation with sodium hydroxide for quantitation oftrans-p-hydroxycinnamic acid and totaltrans-p-hydroxycinnamic acid esters in the leaves ofL. robustumwas developed, since it was difficult and troublesome to analyze no less than 34trans-p-hydroxycinnamic acid esters by usual HPLC. The extract ofL. robustumwas hydrolyzed with sodium hydroxide at 80 °C for 2 h, and then, hydrochloride was added. HPLC analysis was performed in reverse phase mode using a C-18 column, eluting with methanol-0.1% acetic acid aqueous solution (40:60,v/v) in isocratic mode at a flow rate of 1.0 mL·min−1and detecting at 310 nm. The linear range fortrans-p-hydroxycinnamic acid was 11.0–352.0 μg·mL−1(r2= 1.000). The limit of detection and limit of quantification were 2.00 and 6.07 μg·mL−1, respectively. The relative standard deviations of intra-day and inter-day variabilities fortrans-p-hydroxycinnamic acid were less than 2%. The percentage recovery oftrans-p-hydroxycinnamic acid was 103.3% ± 1.1%. It is the first HPLC method using hydrolyzation for quantification of many carboxylic esters. Finally, the method was used successfully to determinetrans-p-hydroxycinnamic acid and totaltrans-p-hydroxycinnamic acid esters in various extracts of the leaves ofL. robustum. The 60–70% ethanol extracts ofL. robustumshowed the highest contents of freetrans-p-hydroxycinnamic acid (3.96–3.99 mg·g−1), and the 50–80% ethanol extracts ofL. robustumdisplayed the highest contents of totaltrans-p-hydroxycinnamic acid esters (202.6–210.6 mg·g−1). The method can be applied also to the quality control of the products ofL. robustum.Keywords:trans-p-hydroxycinnamic acid;esters;Ligustrum robustum;HPLC-UV;hydrolyzation;sodium hydroxide;quantification
研究领域:
植物化学
·
分析化学
·
药用植物研究
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MICROCHIMICA ACTA
·
2018
·Vol. 185
·期 3
·1-9
·
IF 5.705
Ji Shunli,Li Tengfei,Yang Wen,Shu Chang,Li Duo,Wang Yan,Ding Li
A hollow porous molecularly imprinted polymer (HPMIP) is described for use in dispersive solid phase extraction of macrolide antibiotics (MACs). The HPMIP was prepared by using spiramycin as the template, methacrylic acid as the functional monomer, and mesoporous MCM-41 (Mobile Composition of Matter No. 41; with a size of about 100 nm) as a sacrificial support. The sorbent was characterized by Fourier transform infrared spectrometry, transmission electron microscopy, nitrogen adsorption and thermo-gravimetric analysis. Several parameters affecting the extraction efficiency were optimized. The material has a large surface area (359 m 2 ·g −1 ), and most recognition sites are located on the surface of the HPMIPs. This results in high binding capacity (120 μmol·g −1 ) and fast binding (20 min) in comparison to either MCM-41-core surface MIPs or solid MIPs. The method was applied to the extraction of the MACs azithromycin, spiramycin, tilmicosin, tylosin, clarithromycin, roxithromycin and josamycin from spiked honey. The recoveries, determined by HPLC-MS/MS, ranged from 88.0% to 117% at the three spiking levels tested (1, 5 and 20 μg·kg −1 ). Intra-day and inter-day assay precision at three spiking levels are <10.7% (for n = 6) and 12.6% ( n = 3), respectively. The limits of detection are between 3 and 17 ng·kg −1 . This indicates the superiority of the method in selective extraction of macrolides even from complex matrices.
Hollow porous molecularly imprinted polymers using spiramycin as the template are shown to be viable dispersive solid phase extraction adsorbents for selective enrichment of macrolide antibiotics in honey products prior to their quantitation by HPLC-MS/MS.
研究领域:
分析化学
·
食品科学
✓ 已验证
DOI
PubMed
高影响因子
INDUSTRIAL CROPS AND PRODUCTS
·
2024
·
IF 5.6
Weikang Shen,Haobo Wang,Zhouzhe Lan,Guangzhi Xu,Qinxue Ni,Qiufen Mo,Youzuo Zhang,Yan Wang
Gardenia fruit oil (GFO) is a new emerging edible woody oil with few investigations of its’ refinement process. In this study, different degumming, deacidification and bleaching technologies were introduced for realizing moderate refining of the GFO based on the preservation of bioactive micronutrients. Firstly, a simple multi-stage solid phase extraction (SPE) combined with a lab- affordable HPLC-UV instrument was developed for determinations of several vital biological constituents, such as crocetin, geniposide, polyphenols, phytosterols and squalene in the GFO. Satisfactory limit of detection (LOD), limit of quantification (LOQ), recovery, intra-day and inter-day precision were obtained. Subsequently, changes of those phytochemicals during three types of degumming, followed by three kinds of deacidification and then three ways of bleaching were investigated, offering insightful suggestions for achieving moderate refining of the GFO. Finally, the refined GFO might be suggested as a potential functional edible oil with valuable micronutrients. To our knowledge, this is the first study investigating moderate refinement techniques for GFO, as well as developing novel methods for phytonutrients analysis in the GFO.
研究领域:
食品科学
·
分析化学
·
植物化学
✓ 已验证
产品关联
DOI
高影响因子
FOOD CHEMISTRY
·
2021
·
IF 7.514
Lele Yang,Sijia Wu,Jinchao Wei,Jiagang Deng,Xiaotao Hou,Erwei Hao,Lei Zhang,Peng Li
Glucose is a primary source of energy used in most organisms. Thus, development of reliable approaches to measure intracellular glucose uptake is an important research issue. 2-[N-(7-nitrobenz-2-oxa-1,3-diazol-4-yl) amino]-2-deoxy- d -glucose (2-NBDG), as a fluorescent glucose derivative, has been widely used to track intracellular glucose uptake by fluorescence imaging and measuring in mammalian cells. However, the avoid-less cross-interference of intrinsic autofluorescence background and tested fluorescent compounds limits its ability to provide trustworthy information on intracellular glucose uptake. By the extraction, separation and detection of 2-NBDG, a simple, sensitive and accurate HPLC-FLD method was established and validated for the measurement of intracellular glucose uptake in HepG2 cells. The developed method has been employed successfully to assess the glucose uptake activity of anti-diabetic drugs and fluorescent natural products. A fit-for-purpose partial validation was further performed for quantification and comparison of glucose uptake in AML12, LO2 hepatocytes, L6 myoblasts and 3T3-L1 preadipocytes.
研究领域:
分析化学
·
药理学
·
细胞生物学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2024
·
IF 3.1
Xinran Zhang,Mohamed Abdulbagi,Limin Wang,Jiafeng Wang,Bin Di,Bo Li
Amino acid epimerization , a process of converting L -amino acids to D -amino acids, will lead to modification in the protein structure and, subsequently, its biological function . This modification causes no change in protein m/z and may be overlooked during protein analysis . Aspartic Acid Epimerization (AAE) is faster than other amino acids and could be accelerated by free radicals and peroxides. In this work, a novel and site-specific HPLC method using a chiral stationary phase for determining the AAE in the active site model peptide (AP) of Peroxiredoxin 2 has been developed and validated. The developed method showed good linearity (1 – 200 μg/mL) and recoveries of the limit of quantification (LOQ), low, medium, and high concentrations were between 85% and 115%. The Kinetics of AAE in AP were studied using the developed method, and the results showed that when ascorbic acid and Cu 2+ coexisted, the AP epimerized rapidly. The AAE extent increased with time and was positively correlated with hydrogen peroxide generation.
研究领域:
生物化学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2024
·
IF 8.5
Xinmiao Wang,Qian Wang,Dong Cai,Jinghan Yu,Xuan Chen,Xu Guo,Peiyong Tong,Xiaoyang Liu,Fawen Yin,Dayong Zhou
HPLC-UV analysis was used to evaluate the enzymatic degradation characteristics of tyrosol acyl esters (TYr-Es) and alkyl gallates (A-GAs). Among various hydrolytic enzymes, TYr-Es can be hydrolyzed by pancrelipase, while A-GAs cannot be hydrolyzed by pancrelipase. Interestingly, carboxylesterase-1b (CES-1b), carboxylesterase-1c (CES-1c) and carboxylesterase-2 (CES-2) are able to hydrolyze TYr-Es and A-GAs, and thus to liberate tyrosol (TYr) and gallic acid (GA). By contrast, the degrees of hydrolysis (DHs) of TYr-Es and A-GAs by CES-1b and CES-1c were significantly higher than those by CES-2. Meanwhile, the DHs of TYr-Es were much higher than those of A-GAs. Especially, the DHs firstly increased and then decreased with the increasing alkyl chain length. Besides, DHs positively correlated with the unsaturation degree at the same chain length. Through regulating carbon length, unsaturation degree and the ester bond structure, controlled-release of phenolic compounds and fatty acids (or fatty alcohols) from phenolic esters will be easily achieved.
研究领域:
生物化学
·
食品科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Journal of Pharmaceutical Analysis
·
2020
·
IF 2.673
Yuan Hong,Xiaoyan Liao,Zilin Chen
The fruits of leguminous plants Cercis Chinensis Bunge are still overlooked although they have been reported to be antioxidative because of the limited information on the phytochemicals of C. chinensis fruits. A simple, rapid and sensitive HPLC-MS/MS method was developed for the identification and quantitation of the major bioactive components in C. chinensis fruits. Eighteen polyphenols were identified, which are first reported in C. chinensis fruits. Moreover, ten components were simultaneously quantified. The validated quantitative method was proved to be sensitive, reproducible and accurate. Then, it was applied to analyze batches of C. chinensis fruits from different phytomorph and areas. The principal components analysis (PCA) realized visualization and reduction of data set dimension while the hierarchical cluster analysis (HCA) indicated that the content of phenolic acids or all ten components might be used to differentiate C. chinensis fruits of different phytomorph.
研究领域:
药用植物学
·
分析化学
·
植物科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MICROCHIMICA ACTA
·
2023
·Vol. 190
·期 10
·1-13
·
IF 5.7
Bian Yu,Zhang Yuan,Liu Tong,Zhang Feng,Gao Hui-yuan
A novel imine-linked magnetic covalent organic polymer, Fe 3 O 4 @TAB-TFPT, was synthesized using environmentally friendly deep eutectic solvents as the reaction medium instead of conventional organic solvents. The materials were characterized by scanning electron microscope (SEM), transmission electron microscopy (TEM), FT-IR, N 2 adsorption-desorption isotherms, energy dispersive spectrometer (EDS), X-ray photoelectron spectra (XPS), and thermo gravimetric analysis (TGA). Subsequently, the materials were employed as an adsorbent for magnetic solid-phase extraction (MSPE) of flavonoids, including Kurarinone, Norkurarinone, Xanthohumol, and Isoxanthohumol, prior to their determination by HPLC–MS/MS. The validation results demonstrate good linearity within the concentration range 0.1–1000 ng∙mL −1 ( R 2 ≥ 0.9963), high enrichment factors ranging from 18.9 to 30.7, and low LODs (0.01–0.05 ng∙mL −1 ) and LOQs (0.05–0.1 ng∙mL −1 ). Furthermore, recoveries between 80.60% and 108.40% with relative standard deviations ≤ 8.49% were achieved. The proposed MSPE-HPLC–MS/MS method was successfully applied to the determination of flavonoids in Sophora flavescens Aition sample. Graphical Abstract
研究领域:
分析化学
·
材料科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF HAZARDOUS MATERIALS
·
2024
·
IF 12.2
Jinling Pang,Hongzhe Chen,Huige Guo,Kunning Lin,Shuyuan Huang,Beichen Lin,Yuanbiao Zhang
Microplastics (MPs) act as carriers for organic pollutants ( e.g. antibiotics) and microorganisms ( e.g. bacteria) in waters, leading to the proliferation of antibiotic resistance genes. Moreover, the antibiotics adsorbed on MPs may exacerbate this process. For further research, it is necessary to understand the types and amounts of antibiotics adsorbed on MPs. However, due to the heavy work of MPs collection and sample pretreatment, there is a lack of analytical methods and relevant data. In this study, an in-tube solid phase microextraction (IT-SPME) on-line coupled to HPLC-MS/MS method based on amorphous precursor polymer of three-dimensional covalent organic frameworks/monolith-based composite adsorbent was developed, which could efficiently capture, enrich and analyze tetracycline (TCs) antibiotics. Under the optimal extraction parameters, the developed method was capable of detecting TCs at levels as low as 0.48–1.76 pg. This method was applied to analyze the TCs adsorbed on MPs of different particle sizes in mariculture water for the first time, requiring a minimum amount of MPs of only 1 mg. Furthermore, it was observed that there could be an antagonistic relationship between algal biofilm and TCs loaded on MPs. This approach could open up new possibilities for analyzing pollutants on MPs and support deeper research on MPs.
研究领域:
环境科学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MICROCHIMICA ACTA
·
2020
·Vol. 187
·期 6
·1-9
·
IF 6.232
Qin Peige,Zhu Wenli,Han Lizhen,Zhang Xiaowan,Zhao Bing,Zhang Xuebin,Lu Minghua
The monodispersed mesoporous SiO 2 @metal-organic framework (MSN@MIL-101(Fe)) composites were prepared by grafting MSN-NH 2 onto MIL-101(Fe) particles with a solvothermal method. The adsorption ability of the composites was greatly improved compared to that of pristine MSNs or MIL-101(Fe) for phytohormones (Phys). The MSN@MIL-101(Fe) composites were characterized by scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, X-ray diffraction, energy dispersive spectrometer, and mapping analysis. Using MSN@MIL-101(Fe) composites as sorbent, a dispersive solid-phase extraction procedure (dSPE) was developed to extract three endogenous Phys (abscisic acid (ABA), indole-3-aceticacid (IAA), and indole-3-butyric acid (IBA)) and two exogenous Phys (1-naphthylacetic acid (1-NAA) and 2-naphthylacetic acid (2-NAA)) prior to HPLC-DAD analysis. The experimental parameters including sample volume, sorbent amount, adsorption time, adsorption pH, desorption time, and desorption solvent on extraction efficiency were optimized and evaluated. Under optimized conditions, the working range of 0.08 to 0.45 ng mL −1 with enrichment factors from 144 to 207 were achieved. The linear range is 0.75–200 ng mL −1 for IAA, 0.20–200 ng mL −1 for ABA, and 1.0–200 ng mL −1 for IBA, 1-NAA, and 2-NAA. With MSN@MIL-101(Fe) as sorbent for extraction of Phys and determination by HPLC-DAD, two endogenous Phys (IAA and ABA) were detected from mung bean sprouts which were made in a laboratory, and the results were further confirmed by high-resolution mass spectrometry. The composites can be applied to extract other small molecules, which have similar chemical structures with Phys in biological, environmental, and food samples.
Schematic presentation of a dispersive solid-phase extraction using monodispersed mesoporous SiO 2 @metal-organic framework composites (MSNs@MIL-101(Fe)) as the sorbent for extraction, clean-up, and preconcentration of phytohormones in mung bean sprouts prior to HPLC-DAD analysis.
研究领域:
分析化学
·
植物学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
RSC Advances
·
2019
·Vol. 9
·期 12
·6717-6723
·
IF 3.049
Xiuli Dong,Jiayuan Tang,Yan Ren,Xiangming Chen
A novel fluorescence labeling reagent N-acetylhydrazine acridone (AHAD) was designed and synthesized. A highly sensitive high performance liquid chromatography (HPLC) method coupled with fluorescence detection to determine benzaldehyde after derivatization with AHAD was developed. Optimum derivatization was obtained at 40 °C for 30 min with trichloroacetic acid as catalyst. Benzaldehyde derivative was separated on a reversed-phase SB-C18 column in conjunction with a gradient elution and detected by fluorescence detection at excitation and emission wavelengths of 371 nm and 421 nm. The established method exhibited excellent linearity over the injected amount of benzaldehyde of 0.003 to 5 nmol mL−1. The method was successfully applied to the determination of serum semicarbazide-sensitive amine oxidase (SSAO) activity in humans. SSAO is a significant biomarker because serum SSAO activity is elevated in patients with Alzheimer's disease, vascular disorders, heart disease and diabetes mellitus. It was demonstrated that the SSAO activity of the hyperglycemic group (60 ± 4 nmol mL−1 h−1) was significantly higher than that of normal blood sugar group (44 ± 4 nmol mL−1 h−1) with P < 0.05.
研究领域:
分析化学
·
医学
·
生物化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
·
2021
·
IF 5.279
Yong Wang,Wanjun Gao,Yeyun Li,Yu Xiao,Wei Song,Ting Yao,Manhuan Cheng,Wenjuan Wang,Ruyan Hou
The tea shrub is grown in long-standing orchards, an environment that is suitable for persistent weed growth, which is increasingly controlled by herbicides. Therefore, there is increasing concern that tea consumers may be exposed to herbicide residues. In this study, the levels of glufosinate-ammonium (GLU), glyphosate [N-(phosphonomethyl) glycine; PMG], and its metabolite aminomethyl phosphoric acid (AMPA) were determined in tea samples by HPLC–MS/MS using several current purification methods and a new method that we developed herein. The matrix effect of our proposed method was between -27.3 and 27.7%, which was lower than that in other methods, indicating that this method effectively reduced the interference of tea matrix in the mass spectrometry process. This method was used to determine the levels of PMG, GLU, and AMPA in 780 samples, including six traditional Chinese teas (green tea, black tea, oolong tea, dark tea, white tea, and yellow tea) and a floral tea, from 14 provinces of China. Probability estimates showed that the 95th percentile risk entropy values of the three pesticide residues were far below the acceptable risk level. The risk assessment results showed that exposure to PMG, GLU, and AMPA caused by drinking tea beverages poses no significant risk to human health.
研究领域:
分析化学
·
环境科学
·
食品安全
✓ 已验证
产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）