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HPLC-DAD
Analytical Methods · 2017 ·Vol. 9 ·期 17 ·2535-2545 · IF 1.9

Development and validation of green chromatography for the determination of anthocyanins in haskap berry, mulberry and blackberry

Jun Sang,Qun Ma,Cui-qin Li

This study was aimed at developing and validating a green HPLC-DAD method to determine anthocyanins using ethanol and an alpha-hydroxy acid aqueous solution as a mobile phase. The effects of alpha-hydroxy acids on the chromatographic behaviors of cyanidin-3-O-glucoside, the most predominant anthocyanin in nature, in a C18 column were investigated. Among seven selected alpha-hydroxy acids, tartaric acid exhibited potential for improving the chromatographic separation of cyanidin-3-O-glucoside. Cyanidin-3-O-glucoside was the main anthocyanin in haskap berry, mulberry, and blackberry, and the three berries were selected for further method development and validation. The optimized mobile phase was a mixture of ethanol and a 0.25 mol L−1 tartaric acid aqueous solution at the 20 : 80 (v/v) ratio. The retention time of cyanidin-3-O-glucoside was less than 1.8 min, and an optimum separation of anthocyanins was achieved in 4 min. The developed method was validated in terms of linearity, limits of detection and quantification, precision, repeatability, stability, and recovery. The calibration curve revealed good linearity (R2 = 0.9999), and the limits of detection and quantification were 0.038 mg L−1 and 0.125 mg L−1, respectively. The relative standard deviations of intra- and inter-day precision, repeatability, and stability were less than 5%. The recoveries of cyanidin-3-O-glucoside from the berry samples were between 99% and 101%, a satisfactory level. Additionally, the optimized mobile phase had a negligible effect on the C18 column stability. Therefore, the developed method was safe, rapid, and valid for anthocyanin analysis.

研究领域: 分析化学 · 食品科学 · 植物科学
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Chemosensors · 2024 ·Vol. 12 ·期 10 ·220 · IF 3.7

Fast Determination and Source Apportionment of Eight Polycyclic Aromatic Hydrocarbons in PM10 Using the Chemometric-Assisted HPLC-DAD Method

Ting Hu,Yitao Xia,You Wang,Li Lin,Rong An,Ling Xu,Xiangdong Qing

Polycyclic aromatic hydrocarbons (PAHs) are a group of organic compounds that are both toxic and hazardous to human health and ecological systems. In recent work, a novel analytical strategy based on the chemometric-assisted HPLC-DAD method was proposed for the quantification and source apportionment of eight PAHs in PM10 samples. Compared to traditional chromatographic methods, this approach does not require the purification of complex PM10 samples. Instead, it utilizes a mathematical separation method to extract analytes’ profiles from overlapping chromatographic peaks, enabling precise quantification of PAHs in PM10. Firstly, 40 PM10 samples collected in Loudi city during two sampling periods were used for analysis. Subsequently, the second-order calibration method based on alternating trilinear decomposition (ATLD) was employed to handle the three-way HPLC-DAD data. Finally, the pollution sources of PAHs were analyzed by the feature component analysis method according to the obtained relative concentration matrix. For the validation model, the average recoveries of eight PAHs were between (88.8 ± 7.6)% and (105.6 ± 7.5)%, and the root-mean-square errors of prediction ranged from 0.03 μg mL−1to 0.47 μg mL−1. The obtained limits of quantification for eight PAHs were in the range of 0.0050 μg mL−1to 0.079 μg mL−1. For actual PM10 samples, results of the feature component analysis indicated that the main source of PAHs in PM10 may be traffic emissions and coal combustion. In summary, the proposed method provided a new and rapid analysis method for the accurate determination and source apportionment of PAHs in atmospheric aerosols.

研究领域: 环境科学 · 分析化学 · 公共卫生
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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.

研究领域: 食品科学 · 分析化学
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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.

研究领域: 分析化学 · 食品科学 · 环境科学
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Chinese Journal of Natural Medicines · 2019 · IF 1.773

Vitellaria paradoxa nutshells from seven sub-Saharan countries as potential herbal medicines for treating diabetes based on chemical compositions, HPLC fingerprints and bioactivity evaluation

Da LI,Jian-Qi XIAO,Wen-Yuan LIU,Chao-Feng ZHANG,Toshihiro AKIHISA,Masahiko ABE,Eliot-T. MASTERS,Wei-Wei ZHAI,Feng FENG,Jie ZHANG

The aim of the study was to determine the feasibility of the Vitellaria paradoxa nutshell as a new medicinal resource for treating diabetes. A total of forty-one compounds were identified by HPLC-DAD-Q-TOF-MS and phytochemical methods in V. paradoxa nutshell methanol extract. Based on HPLC fingerprints, four characteristic constituents were quantified and the origin of twenty-eight V. paradoxa nutshells from seven sub-Saharan countries was compared, which were classified into three groups with chemometric method. Twenty-eight samples contained high total phenolic content, and exhibited moderate-higher antioxidant activity and strong α -glucosidase inhibitory activity. Furthermore, all fractions and isolated compounds were evaluated for their antioxidant and α -glucosidase inhibitory activities, and α -glucosidase inhibitory action mechanism of four characteristic constituents including protocatechuic acid, 3, 5, 7-trihydroxycoumarin, (2 R , 3 R )-(+)-taxifolin and quercetin was investigated via molecular docking method, which were all stabilized by hydrogen bonds with α -glucosidase. The study provided an effective approach to waste utilization of V. paradoxa nutshell, which would help to resolve waste environmental pollution and provide a basis for developing potential herbal resource for treating diabetes.

研究领域: 药理学 · 药物化学 · 植物科学 · 环境科学
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FOOD CHEMISTRY · 2024 · IF 8.5

Relatively reliable and rapid identification of colorant compounds in food matrices by HPLC-DAD-QTOF-MS combined with theoretical calculation

Jie Shi,Mingquan Huang,Qiang Yang,Yin Xu,Jihong Wu,Hongqin Liu,Jinglin Zhang,Fuping Zheng,Wei Dong

A new convenient method for identifying colorant compounds (CCs) in food matrices was developed using high-performance liquid chromatography with a diode array detector and quadrupole-time-of-flight mass spectrometer (HPLC-DAD-Q/TOF-MS) combined with theoretical calculations. A model sample containing three typical CCs was completely separated via HPLC-DAD. The obtained 3D ultraviolet-visible (UV–vis) spectra revealed the maximum absorption wavelengths (MAWs) of all CCs (yellow, 430 nm; red, 520 nm; blue, 620 nm) in the range of 400–800 nm, and their colors were determined based on their MAWs. Temporary structures of the CCs were obtained using Q/TOF-MS analysis. Theoretical calculations were then performed to obtain the theoretical MAWs and colors of the CCs according to their calculated UV–vis spectra based on temporary structures. The structures of the CCs were confirmed without the need for authoritative standards by comparing the consistency between their experimental and theoretical MAWs and colors. This method is particularly suitable for identifying CCs or compounds with UV–Vis absorption, including new compounds, compounds for which standards are difficult to obtain, and known compounds without reporting relevant molecular information.

研究领域: 食品科学 · 分析化学
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MICROCHEMICAL JOURNAL · 2024 · IF 4.9

Supramolecular solvent for the vortex-assisted dispersive liquid–liquid microextraction of aristolochic acids from Aristolochia debilis prior to HPLC-DAD

Wenxu Hu,Yang Yu,Zhehui Weng,Yao Huang,Yanni Li,Dandan Ge

In this study, a new vortex-assisted dispersive liquid–liquid microextraction technique based on supramolecular solvent (SUPRAS) was proposed for the simultaneous extraction and preconcentration of aristolochic acids (AAs) in Aristolochia debilis followed by HPLC-DAD. A new type of SUPRAS, based on hexafluoroisopropanol (HFIP) and primary amine, with a higher density than water was prepared for the first time. HFIP acted as the coacervation agent and density modifier for the preparation of SUPRAS, and only a small amount of HFIP was required to form the SUPRAS. The influencing parameters such as the type and content of primary amine, the content of HFIP, vortex time, solution pH and ionic strength were thoroughly investigated and optimized. The prepared SUPRAS can effectively exclude macromolecules such as starch and be used to extract AAs from herbal medicines with high extraction efficiency. Under the optimized conditions, the method provided satisfactory linearity (1 ∼ 1000 ng mL −1 for AAb and 10 ∼ 1000 ng mL −1 for AAa with determination coefficients higher than 0.9981), low limits of detection (0.3 ∼ 3.1 ng mL −1 ) and limits of quantification (1.0 ∼ 9.5 ng mL −1 ). In addition, the intra-day and inter-day precision with relative standard deviations (RSDs%) below 6.8 % were obtained. Finally, the proposed method was applied to determine the AAs in Aristolochia debilis , the extraction recoveries were between 92.8 %∼100.6 % with RSDs% between 0.5 % and 7.2 %. Therefore, the developed method was an easy, efficient and reliable method for determining AAs in Aristolochia herbal materials.

CAS / MDL: 111-26-2 111-86-4
研究领域: 分析化学 · 药理学 · 中药学
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FOOD CHEMISTRY · 2012 · IF 3.655

Fast HPLC-DAD quantification of nine polyphenols in honey by using second-order calibration method based on trilinear decomposition algorithm

Xiao-Hua Zhang,Hai-Long Wu,Jian-Yao Wang,De-Zhu Tu,Chao Kang,Juan Zhao,Yao Chen,Xiao-Xia Miu,Ru-Qin Yu

This paper describes the use of second-order calibration for development of HPLC-DAD method to quantify nine polyphenols in five kinds of honey samples. The sample treatment procedure was simplified effectively relative to the traditional ways. Baselines drift was also overcome by means of regarding the drift as additional factor(s) as well as the analytes of interest in the mathematical model. The contents of polyphenols obtained by the alternating trilinear decomposition (ATLD) method have been successfully used to distinguish different types of honey. This method shows good linearity ( r   >   0.99), rapidity ( t   <   7.60   min) and accuracy, which may be extremely promising as an excellent routine strategy for identification and quantification of polyphenols in the complex matrices.

研究领域: 分析化学 · 食品科学
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EUROPEAN FOOD RESEARCH AND TECHNOLOGY · 2020 ·Vol. 246 ·期 10 ·1909-1918 · IF 2.366

Chemometrics-enhanced HPLC–DAD as a rapid and interference-free strategy for simultaneous quantitative analysis of flavonoids in Chinese propolis

Zhang Xiao-Hua,Ma Yi-Xin,Yi Chong,Qing Xiang-Dong,Liu Zhi,Zheng Jing-Jing,Lin Fang,Lv Tian-Feng

In this paper, the application of chemometrics coupled with high-performance liquid chromatography-diode array detection (HPLC–DAD) for the rapid and sensitive quantitative analysis of seven flavonoids in the raw and purified propolis samples was investigated. The objective of this paper was to receive a successful resolution of the complex propolis matrix with minimum experimental time (3.5 min) when appearing unknown interferences, highly overlapping peaks, time and baseline drifts among chromatograms. First, the validation samples contained seven flavonoids at five levels, helped to understand and interpret the features of the second-order calibration method based on the alternating trilinear decomposition (ATLD) algorithm. Second, the experimental data were studied for the simultaneous determination of flavonoids in the raw and purified propolis samples using the function of "mathematical separation" of ATLD algorithm. Except for myricetin (MY), the average recoveries of other analytes were 95.79–105.82% for the raw propolis samples, 94.41–108.06% for the purified propolis samples. In addition, the limit of detection (LOD, 0.01–0.20 μg mL −1 ), limit of quantification (LOQ, 0.03–0.60 μg mL −1 ), sensitivity (SEN, 15.97–184.31 mL μg −1 ), selectivity (SEL, 0.16–0.76) and root-mean-squared error of prediction (RMSEP, 0.29–1.64 μg mL −1 ) of the proposed method, demonstrated that all the target analytes have good sensitivity, low detection limit. According to the experimental results, the total content of flavonoids in purified propolis is about twice that in raw propolis, which is consistent with the actual situation. This analytical strategy will be extremely promising for the identification and quantification of analytes studied in the complex samples.

研究领域: 分析化学 · 植物化学
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FOOD CHEMISTRY · 2021 · IF 7.514

Rapid determination of seven synthetic dyes in casual snacks based on packed-fibers solid-phase extraction coupled with HPLC-DAD

Qing Han,Ying Sun,Kangwei Shen,Yan Yan,Xuejun Kang

Based on packed-fiber solid-phase extraction and HPLC-DAD, a simple analytical method for the determination of seven synthetic dyes has been successfully developed. Polystyrene/polypyrrole (PS/PPy) fibers were obtained via electro-spinning of polystyrene skeletal nanofibers , followed by the oxidation with FeCl 3 to trigger the polymerization of pyrrole and the deposition of polypyrrole coatings on PS fibrous skeleton fibers. The relationship between the extraction performance of the fibers and the electrospinning process at different humidities was investigated based on morphologic study and BET surface area. In the extraction process, purification , concentration, and desorption could be accomplished in one step. The established method exhibited good sensitivity, selectivity, reproducibility, and good efficiency for synthetic dyes in casual snacks (preserved fruit, flavored yogurt, and fruity hard candy) samples. With optimal conditions, the LODs (S/N = 3) were 2.4 to 21.09 ng mL −1 , and linearities were acceptable in liquid matrix and solid matrices. The recoveries were 93.9–103.9%.

研究领域: 分析化学 · 食品科学
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Food Analytical Methods · 2022 ·Vol. 16 ·期 2 ·386-400 · IF 3.498

Fast Quantitative Determination of Principal Phenolic Anti-oxidants in Rosemary Using Ultrasound-Assisted Extraction and Chemometrics-Enhanced HPLC–DAD Method

Xie Lixia,Li Zhineng,Li Haitao,Sun Jiayu,Liu Xueying,Tang Jianxin,Lin Xizhu,Xu Laijun,Zhu Yuefang,Liu Zhi,Wang Tong

Rosemary is an essential source of natural antioxidants, and its extracts have been practised as a preserving agent in foods. A simple, fast, and efficient quantitative determination of principal phenolic antioxidants in rosemary with efficient sample preparation is of great importance for evaluating the quality of rosemary scientifically. This paper presented a chemometrics-enhanced high-performance liquid chromatography with photodiode-array detector (HPLC–DAD) method for simultaneous determination of rosmarinic acid (RA), carnosol (CAR), and carnosic acid (CA) in ultrasound-assisted rosemary extracts. After ultrasound-assisted extraction, the chromatographic procedure in less than 10 min performed with UV detection in the range of 200–390 nm. The alternating trilinear decomposition algorithm in second-order calibration has been applied in extracting relevant qualitative and quantitative information from the three-dimensional chromatographic data. The correlations between the recovered spectra and their normalized pure spectra for RA, CAR, and CA were 0.9906, 0.9988, and 0.9998, respectively. The average recoveries for RA, CAR, and CA were 94.1 ± 3.1%, 92.1 ± 4.1% and 91.8 ± 4.9%, respectively. Due to the second-order advantage, satisfactory resolution and acceptable quantification results were obtained in the presence of overlapping peaks. It expected that this study can provide some valuable references for the simultaneous determination of principal phenolic antioxidants in the quality control of rosemary. Graphical Abstract

研究领域: 食品科学 · 分析化学 · 植物化学
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MICROCHIMICA ACTA · 2022 ·Vol. 189 ·期 12 ·1-10 · IF 6.408

Titania hybridized melamine–formaldehyde aerogel for online in-tube solid-phase microextraction of polycyclic aromatic hydrocarbons prior to HPLC–DAD

Sun Min,Wang Xiuqin,Ding Yali,Feng Juanjuan

In order to improve the selectivity and stability of melamine–formaldehyde (MF) aerogel, it was composited with TiO 2 aerogel. A TiO 2 -MF hybrid aerogel was in situ prepared on the surface of carbon fibers for in-tube solid-phase microextraction (SPME). The extraction performance of TiO 2 -MF aerogel was regulated by changing the ratio of TiO 2 sol and MF sol during the material preparation. Coupled with high-performance liquid chromatography-diode array detection (HPLC–DAD), the extraction tube filled by TiO 2 -MF aerogel-coated carbon fibers was evaluated with several types of environmental pollutants including polycyclic aromatic hydrocarbons (PAHs), estrogens, and ultraviolet filters. Because of favourable extraction performance of PAHs they were selected as model analytes, and some important influence factors were optimized for satisfactory sensitivity. The detection limits were in the range 0.05–0.10 μg L −1 , owing to high enrichment factors (653–1007). The online in-tube SPME-HPLC–DAD method was verified for the determination of trace PAHs in environmental water samples, and acceptable recovery (70–118%) was achieved. The analytical methods also displayed some advantages in comparison with other reports. Moreover, the extraction tube exhibited satisfactory chemical stability. Graphical abstract

研究领域: 分析化学 · 环境科学
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