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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2019 · IF 2.813

Rapid screening and characterization of natural antioxidants in Polygonum viviparum by an on-line system integrating the pressurised liquid micro-extraction, HPLC-DAD-QTOF-MS/MS analysis and antioxidant assay

Zheng-ming Qian,Ling Chen,Meng-qi Wu,De-qiang Li

Rapid discovery of active ingredients from complex matrices is one of great challenges for modern drug development. Traditional methods often require many sample treatment steps, including an extraction step with exclusively dedicated solvents followed by repeated separation and activities assessment. This present work described an integrated analytical setup for natural antioxidants discovery in which the online extraction (OLE) of a solid sample is directly coupled to its analysis by high performance liquid chromatography-diode array detector-quadrupole time-of-flight tandem mass spectrometry and 2,2′-Azinobis-(3-ethylbenzthiazoline-6-sulphonate) (ABTS) antioxidant assay (OLE-HPLC-DAD-QTOF-MS/MS-ABTS). This developed approach makes sample extraction, chromatographic separation and chemical detection, and antioxidant assay integrated into a single HPLC injection and was successfully applied for the rapid discovery of natural antioxidant bioactives from Polygonum viviparum . A total of 21 secondary metabolites were characterized according to their retention times, ultraviolet (UV) spectra, exact mass and fragmentation ions in MS/MS spectra, and 18 of them displayed antioxidant activity (response as negative peaks in antioxidant assay). This work describes a simple, green and efficient approach to minimize the sample consumption (only 0.4 mg was required) and eliminate complex sample treatment procedures. The developed OLE-HPLC-DAD-QTOF-MS/MS-ABTS system offers new perspectives for rapid chemical profiling of natural products and their antioxidants discovery.

CAS / MDL: 64-18-6 7727-21-1
研究领域: 分析化学 · 植物化学 · 药物发现
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FOOD CHEMISTRY · 2020 · IF 6.306

HPLC-DAD fingerprints combined with chemometric techniques for the authentication of plucking seasons of Laoshan green tea

Tian-Qin Peng,Xiao-Li Yin,Hui-Wen Gu,Weiqing Sun,Baomiao Ding,Xian-Chun Hu,Li-An Ma,Shu-Dong Wei,Zhi Liu,Shi-Yi Ye

Laoshan green teas plucked in summer and autumn were measured by high performance liquid chromatography-diode array detector (HPLC-DAD). After baseline correction, the fingerprints data were resolved by multivariate curve resolution-alternating least squares (MCR-ALS) and a total of 57 components were acquired. Relative concentrations of these components were afterwards applied to distinguish plucking seasons using principal component analysis (PCA), support vector machines (SVM) and partial least squares-discriminant analysis (PLS-DA). For both SVM and PLS-DA models, the total recognition rates of training set, cross-validation and testing set were 100%, 91.3% and 100%, respectively. Besides, three variable selection methods were employed to determine characteristic components for the authentication of summer and autumn teas. Results showed that PLS-DA model based on three characteristic components selected by VIP possesses identical predictive ability as the original model. This study demonstrated that our proposed strategy is competent for the authentication of plucking seasons of Laoshan green tea.

研究领域: 分析化学 · 食品科学 · 化学计量学
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Analytical Methods · 2022 ·Vol. 14 ·期 13 ·1329-1334 · IF 3.532

Rapid analysis of triazine herbicides in fruit juices using evaporation-assisted dispersive liquid–liquid microextraction with solidification of floating organic droplets and HPLC-DAD

Beiqi Wu,Yu Niu,Xinyuan Bi,Xiaowen Wang,Liyan Jia,Xu Jing

A rapid and convenient analytical procedure (evaporation-assisted dispersive liquid–liquid microextraction with solidification of floating organic droplets) is advanced for determining the concentrations of triazine herbicide residues (e.g. simazine and atrazine) in fruit juices via HPLC-DAD. The technique involves adding 1-dodecanol (low density) and dichloromethane (high density) to the test solution to act as the extraction and volatile solvents, respectively. Calcium oxide is added to generate heat to accelerate the evaporation of dichloromethane, whereupon the 1-dodecanol quickly disperses into small droplets to complete the microextraction process. Thus, there is no need to use a dispersive solvent and heating equipment is also not required. The floating 1-dodecanol is subsequently frozen using an ice bath to facilitate its separation from the sample. Under optimal conditions (250 μL of 1-dodecanol (extraction solvent), 150 μL of CH2Cl2 (volatile solvent), 1250 mg of CaO, and an extraction time of 60 s) the detection procedure is linear over the range 0.05–5 μg mL−1 (with R > 0.99). The limits of detection (LOD) and quantification (LOQ) were determined to be 0.0022–0.0034 μg mL−1 and 0.0073–0.0113 μg mL−1, respectively. The recovery of simazine and atrazine in three fruit juices ranged between 78.5% and 96.4% with a relative standard deviation <8.2%. Therefore, the proposed approach can be effectively adopted to analyze the triazine herbicide content in fruit juices. The method has been proved to be simple, reliable, and remarkably efficient.

CAS / MDL: 112-53-8 112-42-5
研究领域: 分析化学 · 环境科学 · 食品科学
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INTERNATIONAL JOURNAL OF FOOD SCIENCE AND TECHNOLOGY · 2018 ·Vol. 53 ·期 6 ·1494-1502 · IF 2.383

Development of a green two-dimensional HPLC-DAD/ESI-MS method for the determination of anthocyanins from Prunus cerasifera var. atropurpurea leaf and improvement of their stability in energy drinks

Fang-Fang Chen,Jie Sang,Yao Zhang,Jun Sang

Summary This study aimed to develop a green two-dimensional HPLC-DAD/ESI-MS method for analysing anthocyanins from Prunus cerasifera var. atropurpurea leaf and improve their stability in energy drinks by the addition of phenolic acids. Ethanol and tartaric acid solutions were used as mobile phases for one-dimensional HPLC-DAD for quantitative analysis of anthocyanins, and the primary anthocyanins were identified as cyanidin-3- O -galactoside, cyanidin-3- O -glucoside and cyanidin-3- O -rutinoside using two-dimensional HPLC-MS. Method validation showed that the developed method was accurate, stable and reliable for the analysis of P. cerasifera anthocyanins. The effects of gallic, ferulic and caffeic acid on the stability of cyanidin-3- O -galactoside, cyanidin-3- O -glucoside, cyanidin-3- O -rutinoside and total anthocyanins from P. cerasifera leaf in energy drinks were evaluated, and the degradation of P. cerasifera anthocyanins ideally followed a first-order model ( R 2 > 0.98). Gallic acid showed stronger protective effects on P. cerasifera anthocyanins in energy drinks, and adding/increasing ferulic and caffeic acids accelerated the degradation reactions.

CAS / MDL: 133-37-9
研究领域: 分析化学 · 食品科学 · 植物化学
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ANALYTICAL LETTERS · 2022 · IF 2.267

Determination of 2, 4-Dichlorophenol, 2, 4-Dinitrophenol, and Bisphenol a in River Water by Magnetic Solid-Phase Extraction (MSPE) Using β-Cyclodextrin Modified Magnetic Ferrite Microspheres and High-Performance Liquid Chromatography – Diode Array Detection (HPLC-DAD)

Lanying Xu,Yingying Huang,Bingshan Zhao,Limin Ren,Tao Long

β-Cyclodextrin modified magnetic microspheres were synthesized and used as an effective adsorbent for the solid-phase extraction of three phenols from water samples. Scanning electron microscopy and Fourier transform infrared spectrometry were used to characterize the adsorbents. The major parameters affecting the extraction and desorption efficiencies, such as adsorbent dosage, extraction time, pH, ionic strength, and eluent type were systematically optimized. Under these conditions, three phenols in water samples were extracted and determined by high performance liquid chromatography (HPLC) with diode array detection (DAD). Limits of detection (LODs) of 0.04–0.34 ng mL−1 and limits of quantification (LOQs) from 0.13 to 1.14 ng mL−1 were achieved with good repeatability (relative standard deviation <7.5%). The developed method was applied for the determination of 2,4-dichlorophenol, 2,4-dinitrophenol and bisphenol A in spiked Yangtze River water, and the recoveries were from 81.0% to 94.9%. The results demonstrated that the combination of magnetic solid-phase extraction (MSPE) with HPLC-DAD is suitable for the determination of trace phenolics in environmental water.

CAS / MDL: 10025-77-1 7758-94-3
研究领域: 环境科学 · 分析化学 · 水质分析
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Food Analytical Methods · 2019 ·Vol. 12 ·期 7 ·1674-1683 · IF 2.413

Determination of Four Bitter Compounds in Caramel Colors and Beverages Using Modified QuEChERS Coupled with Liquid Chromatography-Diode Array Detector-Mass Spectrometry

Li He,Wu Chun-Jian,Tang Xiang-Yi,Yu Shu-Juan

The 2,3-dihydro-3,5-dihydroxy-6-methyl-4(H)-pyran-4-one (DDMP), 5-hydroxymethylfurfural (HMF), furfural, and 5-methylfurfural (MF) are the components of caramel colors with intense bitterness. In this study, a practical and simple method for the simultaneous analysis of these four bitter compounds in caramel colors and beverages was proposed using high-performance liquid chromatography–diode array detector–atmospheric pressure chemical ionization–mass spectrometry (HPLC-DAD-APCI-MS). For the sample preparation, the extract efficiencies from different extract solvents and quick, easy, cheap, effective, rugged, and safe (QuEChERS) salt pockets were compared. The correlation coefficients ( R 2 ) of all analytical curves were ≥ 0.9914. The satisfactory recoveries ranged between 70.1% and 101.5%, with relative standard deviations ranged from 1.7% to 9.1%. The matrix effect was evaluated, and HMF, furfural, and MF showed signal enrichment. This method was successfully applied to the analysis of bitter compounds content in several caramel colors and beverages from a local market in China. Four compounds were found in eight samples, with concentration ranging from 0.5 to 1058.1 mg kg −1 .

CAS / MDL: 98-01-1 67-47-0 620-02-0
研究领域: 食品科学 · 分析化学
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Current Analytical Chemistry · 2017 ·Vol. 13 ·期 4 ·317-324 · IF 1.306

A Novel Method for the Analysis of Soluble Carbohydrates from Cistanche deserticola

Guo Yuanheng,Zhao Bing

Objective: A comprehensive monosaccharide quantifying method was developed in this article. Monosaccharides (including glucose, arabinose, galacturonic acid, galactose, mannose, rhamnose and xylose) were analyzed by RP-HPLC-DAD method. Meanwhile, mannitol and fructose were calculated based on peak areas obtained by HPIEC-RID and corresponding data obtained by RP-HPLC-DAD. Monosaccharide compositions of CDSC were analyzed, nine kinds of monosacchardes (glucose, arabinose, galctose, galacturonic acid, mannose, rhamnose, xylose, fructose and mannitol) in were quantified. Background: Cistanche deserticola Y. C. Ma, is a perennial holoparasite and mainly distributed in the desert region of northwestern China. It reported that C. deserticola soluble carbohydrate (CDSC) could prompt lymphocyte proliferation, modulate immunity, inhibit type 2 diabetes, anti-inflammation. For these reasons, it is very appealing to researchers to have a convenient method for monosaccharides analysis of the CDSC. However, previous researches have neglected the faultiness in monosaccharide composition analysis. Therefore, in this study we will focus on establishing a quantifying method of monosaccharides possibly found in C. deserticola. Methods: Soluble carbohydrates were hydrolyzed with trifluoroacetic acid, monosaccharides were labeled with 1-phenyl-3-methyl-5-pyrazolone (PMP), separated by HPLC system equipped with C18 column and detected with DAD (RP-HPLC-DAD). RP-HPLC-DAD method was used for quantitative analysis of glucose, arabinose, galacturonic acid, galactose, mannose, rhamnose and xylose. Meanwhile, hydrolyzates were separated by HPIEC system equipped with aminex HPX-87H ion exclusion column and detected by refractive index detector (HPIEC-RID). The quantity of mannitol and fructose can be calculated based on peak areas obtained by HPIEC-RID and corresponding data obtained by RP-HPLC-DAD. Results: Utilizing this method, monosaccharide compositions of CDSC with different molecular weight (CDCSA, CDCS-B, CDCS-C and CDCS-D) were analyzed, nine kinds of monosacchardes (glucose, arabinose, galctose, galacturonic acid, mannose, rhamnose, xylose, fructose and mannitol) in were found. Conclusion: Fructose and mannitol, which are abundant present in C. deserticola, cannot be analysis by normally PMP modify method, therefore, a comprehensive quantitative analysis method was developed in this research. Galacturonic acid was found out in macro-molecular polysaccharides from C.deserticola, which was not reported before. Galactose and galacturonic acid mainly exist in macro-molecular polysaccharide. Fructose and mannitol mainly exist in mini-molecule or exist in free form.

研究领域: 植物化学 · 分析化学
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Chinese Herbal Medicines · 2014 · IF 0

Rapid Analysis of Polar Components in Ophiocordyceps sinensis by Conventional Liquid Chromatography System

Wen-qing Li,Wen-jia Li,Zheng-ming Qian,Shi-lin Chen,Li Xiang

Objective To develop a rapid high-performance liquid chromatography coupled with diode array detection (HPLC-DAD) method for the simultaneous determination of six polar compounds in Ophiocordyceps sinensis. Methods A poroshell SB Aq column (50 mm × 4.6 mm, 2.7 μm) and gradient elution were used; The detection wavelength of compounds was set at 260 nm. The chromatographic peaks of the six investigated compounds in sample were identified by comparing their retention times with reference compounds. Results All calibration curves showed good linearity ( r > 0.999) within the tested ranges. The intra- and inter-day precisions of the six analytes were less than 0.8% and 2.1%, respectively, and the recoveries of the six analytes were between 95% and 103%. The validated method was successfully applied to the determination of six polar compounds in O. sinensis samples. Conclusion The poroshell SB Aq column is suitable for the rapid analysis of polar components in Chinese materia medica on conventional HPLC system and the developed HPLC method is also helpful to the quality control of O. sinensis .

CAS / MDL: 64-18-6
研究领域: 中药学 · 分析化学
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JOURNAL OF CHROMATOGRAPHY A · 2015 · IF 4.169

Comparison of antioxidant activities of different parts from snow chrysanthemum (Coreopsis tinctoria Nutt.) and identification of their natural antioxidants using high performance liquid chromatography coupled with diode array detection and mass spectrometry and 2,2′-azinobis(3-ethylbenzthiazoline-sulfonic acid)diammonium salt-based assay

L.X. Chen,D.J. Hu,S.C. Lam,L. Ge,D. Wu,J. Zhao,Z.R. Long,W.J. Yang,B. Fan,S.P. Li

Snow chrysanthemum ( Coreopsis tinctoria Nutt.), a world-widely well-known flower tea material, has attracted more and more attention because of its beneficial health effects such as antioxidant activity and special flavor. In this study, a high performance liquid chromatography coupled with diode array detection and mass spectrometry (HPLC-DAD-MS) and 2,2′-azinobis(3-ethylbenzthiazoline-sulfonic acid)diammonium salt (ABTS) based assay was employed for comparison and identification of antioxidants in different samples of snow chrysanthemum. The results showed that snow chrysanthemum flowers possessed the highest while stems presented the lowest antioxidant capacities. Fourteen detected peaks with antioxidant activity were temporarily identified as 3,4′,5,6,7-pentahydroxyflavanone-O-hexoside, chlorogenic acid, 2R-3′,4′,8-trihydroxyflavanone-7-O-glucoside, flavanomarein, flavanocorepsin, flavanokanin, quercetagitin-7-O-glucoside, 3′,5,5′,7-tetrahydroxyflavanone-O-hexoside, marein, maritimein, 1,3-dicaffeoylquinic acid, coreopsin, okanin and acetyl-marein by comparing their UV spectra, retention times and MS data with standards or literature data. Antioxidants existed in snow chrysanthemum are quite different from those reported in Chrysanthemum morifolium , a well-known traditional beverage in China, which indicated that snow chrysanthemum may be a promising herbal tea material with obvious antioxidant activity.

研究领域: 植物化学 · 食品科学 · 药用植物研究
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MOLECULES · 2022 ·Vol. 27 ·期 21 ·7380 · IF 4.927

Simultaneous Extraction and Determination of Characteristic Steroidal Saponins and Homoisoflavonoids in Zhejiang Ophiopogon japonicus

Yaoyao Zhu,Liling Wang,Meixu Chen,Yifeng Zhou,Jun Huang

ZhejiangOphiopogonjaponicus(ZOJ) is a specific variety ofOphiopogon japonicuswith characteristic steroidal saponins and homoisoflavonoids, which are also main pharmacodynamic constituents with clinical effects, including curing inflammation and cardiovascular diseases. However, few analysis methods were applied to simultaneously and quantitatively determine two kinds of its constituents, and hazardous organic solvents are mostly used for extraction. In this study, a new validated simultaneous extraction and determination method for four characteristic steroidal saponins and homoisoflavonoids in ZOJ was established by ionic liquid–ultrasonic extraction (IL-UAE) combined with HPLC-DAD-ELSD analysis, which can be used for the quality control of ZOJ. Chromatographic separation was performed with a DAD wavelength at 296 nm, and the ELSD parameters of the drift tube temperature (DTT), atomizer temperature (AT), and nitrogen gas pressure (NGP) were set at 20% heating power, 70 °C, and 25 psi, respectively. The optimal IL-UAE conditions were 1 mol/L [Bmim]CF3SO3aqueous solution, a liquid–material ratio of 40 mL/g, and an ultrasonic time of 60 min. The proposed method is reliable, reproducible, and accurate, which were verified with real sample assays. Consequently, this work will be helpful for the quality control of ZOJ. It can also present a promising reference for the simultaneous extraction and determination of different kinds of constituents in other medicinal plants.Keywords:ionic liquid (IL);ZhejiangOphiopogonjaponicus(ZOJ);steroidal saponins;homoisoflavonoids;HPLC-DAD-ELSD

研究领域: 药用植物学 · 分析化学 · 药用植物
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Analytical Methods · 2024 · IF 2.7

Zeolitic imidazolate framework-8 as a high-affinity adsorbent for dispersive solid-phase extraction in the analysis of plant growth regulators in fruits

Lian Xia,Can Yuan,Tianqiang He,Jiaxin Cui

Facile and sensitive determination of plant growth regulators (PGRs) in food samples is crucial but still poses a significant challenge. In this study, to enhance the sensitivity of the HPLC-DAD method for PGR detection, a dispersive solid phase extraction (d-SPE) method using zeolitic imidazolate framework-8 (ZIF-8) as the highly effective adsorbent is developed. ZIF-8 nanoparticles are formed through the coordination of Zn2+ with 2-methylimidazole. Due to its high porosity, large surface area, abundant π electronics and nitrogen electronics, ZIF-8 exhibits a strong affinity to PGRs due to the synergistic effects of π–π interaction, van der Waals force, H-bond, and surface effect. Under the optimal d-SPE conditions, the sensitivity of the method is significantly enhanced with outstanding performances, including a wide range of linearity (2.0–200 ng g−1) with high correlation coefficients (R ≥ 0.9989), low limits of detection (LODs, 0.9–8.0 ng g−1 for all PGRs), satisfactory precision (intra-day RSDs ≤ 3.3%, inter-day RSDs ≤ 4.2%), and high accuracy (recovery: 86.6–101.5%). The developed method was successfully applied to quantitatively detect 9 PGRs in fruit samples, yielding satisfactory results. This d-SPE-HPLC-DAD method, characterized by high sensitivity, simplicity, efficiency, ease of practice and cost-effectiveness for PGR detection, shows potential for detecting PGRs in other complex samples and provides a strategy for designing target-affinity adsorbents.

CAS / MDL: 693-98-1 10196-18-6
研究领域: 分析化学 · 食品科学
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CARBOHYDRATE RESEARCH · 2024 · IF 2.4

Sensitive, precise fingerprint profiling for monosaccharide analysis of Bacillus Calmette-Guérin polysaccharide and nucleic acid isolates

Lan Luo,Lisha Lin,Sheng Huang,Yunxi Zhou,Shengmei Yang,Yan Zhu,Lanyan Zhang,Donghua Xiong,Yongsheng Wu,Mingyi Wu

A sensitive and precise HPLC-DAD method with pre-column PMP derivatization was established and validated, for analyzing the polysaccharides in Bacillus Calmette-Guérin polysaccharide and nucleic acid (BCG-PSN) isolates, after acid hydrolysis. And the HPLC fingerprint profiling was used to analyze its monosaccharide composition. The monosaccharide concentration-peak area calibration curve was of good linearity (R 2  > 0.99), over the range of 0.016–0.08 mg/mL for mannose or 0.24–1.20 mg/mL for glucose, with high recovery of 93–105 % for quality control samples. The intra-day RSD values of mannose and glucose concentration were less than 2.5 % and 2.1 %, respectively, and their inter-day RSD values were less than 4.3 % and 2.2 %, respectively, and remained stable for up to 14 days. This method also remained durable against changes in chromatographic parameters, but it's susceptible to the flow rate of mobile phase. Additionally, the method was applied to analyze the content of mannose and glucose in 22 batches BCG-PSN powder and 17 batches BCG-PSN injection. The results showed that the HPLC-DAD fingerprint spectra of all the BCG-PSN powder and BCG-PSN injection samples had a high degree of similarity, with the similar indexes up to 0.999 and 0.998, respectively. The HPLC-DAD method with pre-column PMP derivatization is highly rapid, effective, visual, and accurate for determination of monosaccharide contents. The validated method was successfully applied to the analysis of polysaccharide in both BCG-PSN powder and injection.

CAS / MDL: 89-25-8
研究领域: 生物化学 · 药物分析 · 医学
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