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Food Chemistry-X · 2023 · IF 6.1

Aqueous two-phase systems coupled with chemometrics-enhanced HPLC-DAD for simultaneous extraction and determination of flavonoids in honey

Xiao-Hua Zhang,Xiang-Dong Qing,Jing-Jing Zheng,Yan Yu,Jiaojiao Huang,Chao Kang,Zhi Liu

In this study, an accurate, rapid, green, and environment friendly method for the extraction and quantitative analysis of flavonoids in honey was established by using the aqueous two-phase extraction combined with the chemometrics-assisted HPLC-DAD. The first purpose of this study was to extract seven flavonoids in five different types of honey using alcohol/salt aqueous two-phase system (ATPS). The system with 2.82 mL sodium citrate (30%), 1.58 mL water, and 3.10 mL isopropanol, showed the highest flavonoids extraction yields in the top phase (87.66–101.50%). Additionally, the three-way array of honey samples based on HPLC-DAD was decomposed mathematically by the alternating trilinear decomposition (ATLD) algorithm to obtain reasonable chromatograms, spectra, and concentration profiles for each analyte. Compared with the traditional solid-phase extraction method, the ATPS-ATLD-based method showed satisfactory spiked recoveries, lower limit of detection, and higher sensitivity, further verifying its accuracy and stability.

✓ 已验证 产品关联 DOI PubMed 高影响因子
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TALANTA · 2019 · IF 4.916

Zwitterion-functionalized polymer microspheres-based solid phase extraction method on-line combined with HPLC–ICP-MS for mercury speciation

Xiaoyu Jia,Junyi Zhao,Hongyun Ren,Jiani Wang,Zixiao Hong,Xian Zhang

Zwitterion-functionalized polymer microspheres (ZPMs) have been designed and used as the core adsorbent for the selective and rapid enrichment of mercury species in environmental waters by an on-line solid-phase extraction (SPE). Zwitterionic S-ZPMs and N-ZPMs having an anionic sulfonic group, but differing in cationic S + and N + moieties were prepared from Merrifield resin by treating with 1,2-ethanedithiol and imidazole , followed by modification with 1,3-propanesultone. Without any additional reagents, inorganic mercury (In-Hg), methylmercury (MeHg) and ethylmercury (EtHg) were quantitatively adsorbed on the home-made mini-column packed with ZPMs. Following extraction with 60 mM ammonium acetate and 0.15% L -cysteine ( L -Cys) solution within seconds, separation and speciation of mercury were successfully achieved by the HPLC–ICP-MS technique. Under the optimized experimental conditions, the enrichment factors (EFs) are up to 105 and 98 for inorganic and organic mercury only with 40 mL sample solution, respectively. The low detection limits of 0.78 ng L −1 , 0.63 ng L −1 , and 0.49 ng L −1 were reached for In-Hg, MeHg and EtHg, respectively, with the relative standard deviations (RSDs) below 4.1%. The feasibility and accuracy of the on-line SPE–HPLC–ICP-MS method were successfully applied for mercury speciation in surface water, seawater as well as certified reference material (CRM). The results here demonstrate a facile, sensitive and selective method for speciation of mercury at trace levels.

CAS / MDL: 52-90-4
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Chinese Herbal Medicines · 2019 · IF 0

Monosaccharide analysis and fingerprinting identification of polysaccharides from Poria cocos and Polyporus umbellatus by HPLC combined with chemometrics methods

Jie Liu,Jing Zhou,Qian-qian Zhang,Min-hang Zhu,Mo-li Hua,Yun-hui Xu

Objective Poria cocos and Polyporus umbellatus are similar medicinal fungi in traditional Chinese medicines . A method for fingerprint analysis of monosaccharide composition of polysaccharides by HPLC combined with chemometrics methods has been developed for characterization and discrimination of them in this research. Methods The polysaccharides were extracted by decocting in water, and then completely hydrolyzed with hydrochloride. Monosaccharides in the hydrolyzates were derivatized with 1-phenyl-3-methyl-5-pyrazolone (PMP) for HPLC analysis. More than 20 batches of P. cocos and P. umbellatus from different regions were analyzed. Results The fingerprints of P. cocos showed five common characteristic peaks, which were identified by comparing with the reference substances. The five peaks corresponded to the derivatives of mannose , ribose , glucose, galactose , and fucose . At the same time, the fingerprints of P. umbellatus showed eight common characteristic peaks, of which seven were identified as the derivatives of mannose, ribose, rhamnose , glucose, galactose, xylose , and fucose. Moreover, the similarity of their fingerprints was respectively calculated by the Similarity Evaluation System for Chromatographic Fingerprint of TCM published by China Pharmacopoeia Committee (Version 2004A). And the data were further processed by hierarchical cluster analysis (HCA) and principal component analysis (PCA). The similarity evaluation and HCA indicated that there were no significant difference in P. cocos or P. umbellatus samples from different geographical regions, but PCA was performed to characterize the difference in monosaccharide constituents between P. cocos and P. umbellatus , and linear discriminant analysis (LDA) showed the overall correct classification rate was 100%. Conclusion The fingerprint analysis method of monosaccharide composition of water-soluble polysaccharides can distinguish P. cocos and P. umbellatus , and can be applied for the authentication or quality control for P. cocos and P. umbellatus.

CAS / MDL: 89-25-8
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TALANTA · 2018 · IF 4.244

Screening of a highly effective fluorescent derivatization reagent for carbonyl compounds and its application in HPLC with fluorescence detection

Liu Chen,Yu-Jia Fu,Wen-Le Fang,Xiao-Feng Guo,Hong Wang

Carbonyl compounds are widely distributed in organisms, and the commonly used methods for determination of them like UV/fluorescence/mass spectrometry always require derivatization reagents. However, the reported derivatization reagents have significant difference in reactivity, which is very unfavorable for developing highly reactive reagent. In this study, we theoretically investigated the factors affecting the reactivity of hydrazine-based derivatization reagents, and proposed a strategy for filtering highly reactive reagents by quantum chemical calculation . With this strategy, N-propyl-4-hydrazino-1,8-naphthalimide (NPHNA) was filtered out as a fluorescent derivatization reagent. Taking aliphatic aldehydes as representatives, we evaluated the reactivity of NPHNA for carbonyl compounds. The derivatization of NPHNA with aliphatic aldehydes could be finished at room temperature within 60 min or 35 °C within 35 min, which showed higher reactivity than the most popular UV/MS reagent, 2,4-dinitrophenylhydrazine (DNPH). We believe that the strategy we proposed in this work is of great potential to design highly reactive UV/fluorescent/MS labeling reagents for carbonyl compounds and even other analytes.

✓ 已验证 产品关联 DOI PubMed 高影响因子
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MOLECULES · 2017 ·Vol. 22 ·期 11 ·1927 · IF 2.861

Chemical Fingerprint and Multicomponent Quantitative Analysis for the Quality Evaluation of Cyclocarya paliurus Leaves by HPLC–Q–TOF–MS

Yanni Cao,Shengzuo Fang,Zhiqi Yin,Xiangxiang Fu,Xulan Shang,Wanxia Yang,Huimin Yang

Cyclocarya paliurusis an edible and medicinal plant containing various bioactive components with significant health benefits. A combinative method using high-performance liquid chromatography (HPLC) fingerprint and quantitative analysis was developed and successfully applied for characterization and quality evaluation ofC. paliurusleaves collected from 18 geographical locations of China. For the fingerprint analysis, 21 common peaks were observed among the 18 samples, and these peaks were identified by high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (HPLC–Q–TOF–MS), while a simultaneous quantification of 16 markers was conducted to interpret the variations of contents of these bioactive compounds among theC. paliurusleaves from different geographical locations. Quantification results showed that the contents of these sixteen investigated compounds varied greatly among the leaves from different locations. The developed new method would be a valuable reference for further study and development of this bioactive plant.Keywords:Cyclocarya paliurus;fingerprint;HPLC–Q–TOF–MS;quantitative analysis;quality evaluation

CAS / MDL: 64-18-6
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Analytical Methods · 2022 ·Vol. 14 ·期 25 ·2522-2530 · IF 3.532

A novel magnetic metal–organic framework absorbent for rapid detection of aflatoxins B1B2G1G2 in rice by HPLC-MS/MS

Ling-Juan Wang,Zhi-Wei Chen,Teng-Zhou Ma,Jiang Qing,Fang Liu,Zhou Xu,Ye Jiao,Shi-Hua Luo,Yun-Hui Cheng,Li Ding

In this study, a core–shell-structured magnetic metal–organic framework (MMOF) composite material (Fe3O4@UiO-66-NH2) was synthesized by the solvothermal method. It was employed as a new absorbent in combination with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) for the simultaneous detection of four aflatoxins (AFs) in rice. This method could shorten the pre-processing time by exploiting the advantageous characteristics of magnetic cores. The impurity was removed quickly. The effects of extraction solution, extraction time, adsorbent types, and amount of adsorbent on the extraction rate of target compounds were optimized. Under optimized conditions, AFs were validated and showed a good linear relationship within the 0.375–20 μg kg−1 concentration range (r2 > 0.9992). The limit of detection (LOD) was 0.0188–0.1250 μg kg−1 and the limit of quantification (LOQ) was 0.0375–0.3750 μg kg−1. At three spiking levels (0.375, 2, and 10 μg kg−1), the average recovery values for the four AFs ranged from 85.1% to 111.0%. The relative standard deviation ranged from 3.4% to 7.7%. The new method proved to be simple, fast, efficient, and suitable for the determination of AFs in rice samples.

CAS / MDL: 10025-77-1
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Pharmaceuticals · 2021 ·Vol. 14 ·期 11 ·1194 · IF 5.863

Simultaneous Quantification of Propylthiouracil and Its N-β-d Glucuronide by HPLC-MS/MS: Application to a Metabolic Study

Min Li,Qingfeng He,Li Yao,Xiaofeng Wang,Zhijia Tang,Xiao Zhu,Hai-Shu Lin,Xiaoqiang Xiang

Propylthiouracil (PTU) is commonly prescribed for the management of hyperthyroidism and thyrotoxicosis. Although the exact mechanism of action is not fully understood, PTU is associated with hepatoxicity in pediatric population. Glucuronidation mediated by uridine 5′-diphospho-glucuronosyltransferases (UGTs), which possess age-dependent expression, has been proposed as an important metabolic pathway of PTU. To further examine the metabolism of PTU, a reliable HPLC-MS/MS method for the simultaneous quantification of PTU and its N-β-D glucuronide (PTU-GLU) was developed and validated. The chromatographic separation was achieved on a ZORBAX Extend-C18 column (2.1 × 50 mm, 1.8 μm) through gradient delivery of a mixture of formic acid, methanol and acetonitrile. The electrospray ionization (ESI) was operated in its negative ion mode while PTU and PTU-GLU were detected by multiple reaction monitoring (MRM). This analytical method displayed excellent linearity, sensitivity, accuracy, precision, recovery and stability while its matrix effect and carry-over were insignificant. Subsequently, the in vitro metabolism of PTU was assessed and UGT1A9 was identified as an important UGT isoform responsible for the glucuronidation of PTU. The information obtained from this study will facilitate future mechanistic investigation on the hepatoxicity of PTU and may optimize its clinical application.Keywords:propylthiouracil;propylthiouracil glucuronide;in vitro;human liver microsomes;UGT1A9;HPLC-MS/MS

CAS / MDL: 51-52-5
✓ 已验证 产品关联 DOI PubMed 高影响因子
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Foods · 2021 ·Vol. 10 ·期 11 ·2814 · IF 4.35

Simultaneous Determination of Purines and Uric Acid in Chinese Chicken Broth Using TFA/FA Hydrolysis Coupled with HPLC-VWD

Manli Wu,Wangang Zhang,Xixi Shen,Wei Wang

Chinese chicken broth is well known for its outstanding nutritional value and flavor, widely consumed in China. This study was designed to develop a sensitive and accurate high-performance liquid chromatography-variable wavelength detector (HPLC-VWD) method to simultaneously determine purines and uric acid in Chinese chicken broth for gout and hyperuricemia dietary management. Chromatographic separation was performed on an Agilent TC-C18 (2) column (4.6 mm × 250 mm, 5.0 µm), using 0.02 M KH2PO4(pH 4.0) as a mobile phase. Sample pretreatment was optimized to enable the extraction of all analytes from Chinese chicken broth. The optimal pretreatment conditions were chicken broth-60% trifluoroacetic acid (TFA)/20% formic acid (FA) (1:1,v/v) in a volume ratio of 1:3 and hydrolysis for 40 min at 85 °C in a water bath. The limits of detection (LODs) and limits of quantification (LOQs) of the purines and uric acid were 0.58–1.71 µg/L and 1.92–5.70 µg/L, respectively. The recoveries were 91–101%, with the relative standard deviations (RSDs) lower than 3%. The complete method has been successfully applied to determine purines and uric acid in various Chinese chicken soups obtained from different provinces in China.Keywords:Chinese chicken broth;purine;uric acid;HPLC;acid hydrolysis;hyperuricemia;gout

CAS / MDL: 64-18-6 76-05-1
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Arabian Journal of Chemistry · 2021 · IF 5.165

HPLC-Q-Orbitrap-MS/MS phenolic profiles and biological activities of extracts from roxburgh rose (Rosa roxburghii Tratt.) leaves

Ruimin Wang,Ruiping He,Zhaohui Li,Xue Lin,Lu Wang

Rosa roxburghii Tratt. leaves (RRLs) have been exploited as a alternative tea product in China owing to its various biological properties. A comparative study was performed for the first time on high-performance liquid chromatography quadrupole orbitrap tandem mass spectrometry (HPLC-Q-Orbitrap-MS/MS) phenolic profiles, antioxidant, α -glucosidase inhibitory ( α -GIA) and anti-bacterial activities of the RRLs extracts extracted by traditional and eco-friendly solvents. The RRLs extracts extracted with four screened deep eutectic solvents (DES) showed higher total phenolic content (TPC, 167.48–190.14 mg GAE/g DW) and moderate total flavonoid content (TFC, 3.78–4.11 mg RE/g DW), while the RRLs extracts extracted with choline chloride-1,2-propanediol, choline chloride-levulinic acid, and 50% methanol/ethanol extracts had the highest TFC. Ethyl acetate extracts had the lowest TPC and TFC. Additionally, the phenolic constituents of the RRLs extracts were identified and quantified via HPLC-Q-Orbitrap-MS/MS and HPLC-DAD methods. A total of 30 phenolic compounds were identified in RRLs extracts. Among them, arbutin, gallic acid, (+)-catechin, 3-hydroxybenzoic acid, quercetin-3- O -galactoside and myricetin were the representative ones. The selected DES (especially for choline chloride-lactic acid and choline chloride-levulinic acid) extracts exhibited higher 2,2′-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid (ABTS +• ) and 2,2-diphenyl-1-picrylhydrazyl (DPPH • ) scavenging activities, cupric reducing antioxidant capacity (CUPRAC), ferric reducing antioxidant power (FRAP) except for reducing power, α -GIA and anti-bacterial activity as compared with the extracts extracted with other solvents. Multivariate analysis results revealed that the extraction solvents significantly affected the phenolic constituents and biological activities of the RRLs extracts. The present study presented eco-friendly solvents for high-efficient extraction of the phenolic metabolites from RRLs. RRLs as a potential source enriched in phenolic constituents can be applied in the health, cosmetic and pharmaceutical industries.

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Food Analytical Methods · 2021 ·Vol. 14 ·期 11 ·2375-2385 · IF 3.366

Magnetic Solid-Phase Extraction Followed by HPLC–DAD for Highly Sensitive Determination of Phthalate Esters in Edible Vegetable Oils

Zhao Yuanli,Zhu Zhenbao,Liu Jianghua,Liu Jichao,Li Guoliang

Phthalate esters (PAEs) are prone to migrate from the plastic containers into oil during production and storage process. Owing to the trace amount of PAEs and complex sample matrix, it is of great importance to explore a facile and sensitive way to extract and detect PAEs from oil samples. In this work, magnetic covalent organic framework nanospheres (Fe 3 O 4 @COF(TbBD)) were fabricated by the aldehyde-amine condensation between benzidine (BD) and 1,3,5-triformylbenzene (Tb) on the surface of Fe 3 O 4 nanoparticles with the help of ultrasonic treatment. The new type nanomaterials were firstly used to the magnetic solid-phase extraction (MSPE) of seven PAEs in edible vegetable oils prior to high performance liquid chromatography coupled with a diode array detector (HPLC–DAD). In order to achieve the best extraction efficiency, several key parameters were optimized. Under optimal conditions, the proposed Fe 3 O 4 @COF(TbBD)-MSPE-HPLC–DAD method possessed high sensitivity (0.55–0.95 µg/kg for LODs and 1.80–3.10 µg/kg for LOQs), good linearity ( R 2  ≥ 0.9983), and satisfactory recoveries (80.2–102.9%). The RSDs for intra-day was less than 6.1%, and inter-day was less than 7.9%. This work not only proposed a rapid and reliable approach for determining PAEs in edible vegetable oils but also broadened the application of magnetic COFs in food determination.

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MOLECULES · 2020 ·Vol. 25 ·期 2 ·344 · IF 3.267

Simultaneous Determination of Six Isoflavones from Puerariae Lobatae Radix by CPE-HPLC and Effect of Puerarin on Tyrosinase Activity

Limin Qu,Ke Song,Qi Zhang,Jie Guo,Juan Huang

Tyrosinase inhibitors with excellent inhibitory activities and lower side effects have promising applications in the fields of medicine, agriculture, food sciences and cosmetics. In this study, a method for simultaneous separation and determination of six target compounds (puerarin, daidzin, genistein, daidzein, genistin, and formononetin) inPuerariae LobataeRadix was established by cloud point extraction (CPE) and concentration combined with high performance liquid chromatography (HPLC). To achieve high extraction yields, an ultrasound-assisted extraction method was developed based on a salt-modified Triton X-100 system. The optimal extraction conditions are: surfactant Triton X-100 concentration 0.07 g/mL, liquid-solid ratio 80:1 (mL/g), NaCl addition amount 0.6 g, equilibrium time 40 min, equilibrium temperature 70 °C. Under the optimal conditions, the total maximum extraction yield of the six target isoflavones reached 8.92 mg/g. Usingl-tyrosine andl-dopa as substrates, the effects of puerarin on the monophenolase and diphenolase activity of tyrosinase activity were investigated by the enzyme kinetics method. The results showed that puerarin inhibited monophenolase activity with an IC50of 0.537 mg/mL and activated diphenolase activity. The inhibition type of puerarin on monophenolase and the activation type of puerarin on diphenolase were analyzed by Lineweaver-Burk plots which show that puerarin showed mixed inhibition on monophenolase and mixed activation on diphenolase. Therefore, puerarin can be used as both a tyrosinase inhibitor and a tyrosinase activator.Keywords:Puerariae LobataeRadix;cloud point extractions;tyrosinase inhibitors;tyrosinase activator;kinetic analysis

✓ 已验证 产品关联 DOI PubMed 高影响因子
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TALANTA · 2019 · IF 4.916

Magnetic hyperbranched molecularly imprinted polymers for selective enrichment and determination of zearalenone in wheat proceeded by HPLC-DAD analysis

Yan Zhang,Donghao Liu,Jun Peng,Yanru Cui,Yi Shi,Hua He

A novel magnetic surface molecular imprinted polymers with 2, 4, 6-trisacrylamido-3, 5-triazine (TAT) as a functional monomer was successfully synthesized and used for the enrichment and determination of zearalenone . The molecular imprinting is reported herein at first time for application of zearalenone in wheat. The magnetic imprinted materials possessed excellent magnetism and uniform appearance, which were characterized by fourier transform infared spectroscopy and transmission electron microscope. The results proved the magnetic molecular imprinted polymers was successfully prepared. The magnetic molecular imprinted polymers exhibited satisfactory sensitivity, stability and potential reusability. The binding affinity was investigated by selectivity experiment, which possessed high selectivity. To obtain the optimal application conditions, the amount of adsorption, extraction time, elution solvent and time were optimized. The limited detection of zearalenone was 0.55 ng g −1 and the recoveries of zearalenone were 92.1–96.0%. The relative standard deviation was lower than 5.4%. This indicated that a simple, efficient and low-cost method was established and successfully applied in spiked wheat sample.

CAS / MDL: 78-67-1
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