FOOD CHEMISTRY
·
2022
·
IF 9.231
Yi Zhang,Zhi-Liang Yuan,Xin-Yu Deng,Hao-Dong Wei,Wen-Long Wang,Zhenghua Xu,Yongwei Feng,Xueli Shi
The residues of bisphenol A (BPA) in milk packaging may transfer to milk, adversely affecting the human endocrine system. Consequently, to analyse or monitor BPA, it is imperative to develop rapid and effective approaches to BPA extraction from milk and milk packing as BPA is usually present in trace levels. Herein, we developed a rapid, simple, and low-cost dispersive-membrane-solid-phase-extraction (DME) for BPA with MIL-101(Cr) mixed-matrix-membrane (MMM). The MMM had large surface area (1322.09 m 2 /g) and pore volume (0.65 cm 3 /g), possessed great extraction efficiency of BPA, and kept more than 90% extraction efficiency after 20 times of reuse. Using the developed MIL-101(Cr)-MMM-based DME coupled with HPLC-fluorescence detector, we received an adequate linearity in the range of 0.1 ∼ 50 μg/L BPA and a limit of detection as low as 16 ng/L under optimized conditions. The recoveries of BPA in milk and milk bottles were from 74.2% to 110.6%, with RSDs less than 9.4%.
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JOURNAL OF PHARMACY AND PHARMACOLOGY
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2022
·Vol. 74
·期 7
·1040-1050
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IF 4.81
Zhang Sijie,Gong Xingchu,Qu Haibin
ObjectivesTo investigate the feasibility of using near-infrared spectroscopy for rapid determination of main organic acids in Ginkgo biloba leaf extract (EGBL).MethodsMain organic acids in EGBL were assayed using the HPLC method. Critical factors of the chromatographic separation were optimized by a novel analytical quality by design approach. Partial least squares-discriminant analysis (PLS-DA) was performed to screen the marker components, and principal component analysis (PCA) was utilized to distinguish the different samples. Then, spectral quantification potential was investigated using PLS and support vector machine (SVM) approaches. For modelling, different spectral preprocessing and wavelength selection methods were systematically compared.Key findingsIt was found that quinic acid, protocatechuic acid and 6-hydroxykynurenic acid were identified as possible index components. PLS-DA based on contents and PCA based on near-infrared spectra can both effectively distinguish the different EGBL samples. The calibration models with wonderful prediction performance can be both developed by the PLS and SVM algorithms.ConclusionsNIR spectroscopy combined with chemometrics can realize the rapid and non-destructive qualitative and quantitative analysis of EGBL. The proposed method may be applied to quality control of EGBL and other natural products in commercial use.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2022
·
IF 3.571
Mengmeng Song,Xianjie Sheng,Genyi Ye,Zhuicheng Xu,Xinru Li,Tong Xie,Haishan Deng,An Kang
Gut microbiota-derived tryptophan (TRP) metabolites, especially the indole derivatives, function as critical modulators of intestinal immune function and integrity via modulating the aryl hydrocarbon receptor pathway. Selective enrichment of these indole metabolites in biological samples is important for quantitative determination by routine methods such as HPLC. Here, we report a molecularly imprinted polymer (MIP) for solid-phase extraction (SPE) of TRP-derived indole metabolites from faeces of mice. The MIP was synthesized by surface polymerization by using indole-3-acetic acid (IAA) and acrylamide after cross-linking by ethylene glycol dimethacrylate (EGDMA) and initialed by 2′,2-azobisisobutyronitrile (AIBN). The MIPs were then characterized by transmission electron microscope (TEM) and fourier transform infrared spectroscopy (FTIR), and the adsorption capacity, selectivity and reusability of MIPs were systematically evaluated. Results showed that IAA-MIPs showed a uniformly distributed nanoshell layer with a thin shell thickness of 26 nm . The IAA-MIPs could selectively adsorb IAA, indole-3-propionic acid (IPA), and indole-3-lactic acid (ILA) in a mixed solution that also contains TRP and tyrosine. The adsorption capacity of IAA-MIPs only slightly decreased with the increase of recycling use. As purification material for SPE, the IAA-imprinted polymers (IAA-MIPs) were successfully applied to extract IAA, IPA, and ILA from normal and colitis mice for HPLC determination. Collectively, these surface molecularly imprinted polymers could find extensive use to selective enrichment of microbiota-derived indole metabolites in biological samples.
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MOLECULES
·
2023
·Vol. 28
·期 10
·4170
·
IF 4.6
Jing Chen,Qi Huang,Zhuobin He,Guoying Tan,Yuansheng Zou,Juying Xie,Zhengming Qian
Polygoni Cuspidati Rhizoma et Radix (PCR), the rhizome and root ofPolygonum cuspidatumSieb. et Zucc., has been used as an herbal medicine for a long time. In this study, the ultrafiltration combined with high performance liquid chromatography (UF-HPLC) method was developed to screen tyrosinase (TYR), α-glucosidase (α-GLU), and xanthine oxidase (XOD) inhibitors from PCR. Firstly, the inhibitory activity of 50% methanol PCR extract on TYR, α-GLU, XOD, and acetylcholinesterase (ACHE) was tested. The extract showed a good inhibition on the enzymes, except for ACHE. Therefore, UF-HPLC experiments were carried out to screen TYR, α-GLU, and XOD inhibitors from PCR extract. Seven potential bioactive components were discovered, including methylgallate (1), 1,6-di-O-galloyl-D-glucose (2), polydatin-4′-O-D-glucoside (3), resveratrol-4′-O-D-glucoside (4), polydatin (5), malonyl glucoside resveratrol (6), and resveratrol-5-O-D-glucoside (7). Most of them were found as enzyme inhibitors from PCR for the first time, except polydatin (5), which had been reported as an α-GLUI in PCR in the literature. Finally, molecular docking analysis was applied to validate the interactions of these seven potential active components with the enzymes. Compounds1–7were proven as TYR inhibitors, compounds2,4–7were identified as XOD inhibitors, and compounds4–6were confirmed as α-GLU inhibitors. In short, the current study provides a good reference for the screening of enzyme inhibitors through UF-HPLC, and provides scientific data for future studies of PCR.Keywords:Polygoni Cuspidati Rhizoma et Radix;enzyme inhibitor;tyrosinase;xanthine oxidase;α-glucosidase;ultrafiltration
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2023
·Vol. 415
·期 17
·3375-3384
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IF 4.3
Liu Si,Lu Boling,Peng Zijuan,Liu Chunyu,Liu Yuhui,Jiao Hui,Wu Dan,Li Penghui,Zhao Xingchen,Song Shanjun
In organic purity assessment, chromatography separation with a suitable detector is required. Diode array detection (DAD) has been a widely used technique for high-performance liquid chromatography (HPLC) analyses, but its application is limited to compounds with sufficient UV chromophores. Charged aerosol detector (CAD), as a mass-dependent detector, is advantageous for providing a nearly uniform response for analytes, regardless of their structures. In this study, 11 non-volatile compounds with/without UV chromophores were analyzed by CAD using continuous direct injection mode. The RSDs of CAD responses were within 17%. For saccharides and bisphenols, especially, the RSDs were lower ( 2.12% and 8.14%, respectively). Since bisphenols exist in UV chromophores, their HPLC–DAD responses were studied and compared with CAD responses, with CAD showing a more uniform response. Besides, the key parameters of HPLC-CAD were optimized and the developed method was verified using a Certified Reference Material (CRM, dulcitol, GBW06144). The area normalization result of dulcitol measured by HPLC-CAD was 99.89% ± 0.02% ( n = 6), consistent with the certified value of 99.8% ± 0.2% ( k = 2). The result of this work indicated that the HPLC-CAD method could be a good complementary tool to traditional techniques for the purity assessment of organic compounds, especially for compounds lacking UV chromophores. Graphical Abstract
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Chinese Journal of Natural Medicines
·
2021
·
IF 3
Zheng-Ming QIAN,Zi WU,Qi HUANG,Chuan-Xi WANG,Guo-Yin TAN,Wen-Jia LI,Wan-Yang SUN,Gen-Pin LV,Hao GAO
An eco-friendly and fast HPLC method was developed for the determination of adenosine, inosine, guanosine and uridine in Cordyceps and related products (fermented mycelia of Hirsutella sinensis and Paecilomyces hepiali ). The sample was ultrasonically extracted using 0.5% phosphoric acid solutions for 2.5 min. Sample separation was performed on a Poroshell SB-Aq column (50 mm × 4.6 mm, 2.7 μm) using eco-friendly mobile phase consisting of formic acid and ammonium formate aqueous solution at a flow rate of 1.0 mL·min −1 . The detection wavelength was 260 nm. The developed HPLC method showed good linearity with correlation coefficients of 1.0000 in the test range. Good precision, repeatability and stability of this method were also observed (RSD ≤ 2.81%). The recovery ranged from 91.84%−105.19% (RSD ≤ 2.59%). Compared with reported methods, the current method did not use harmful organic solvent and took only 10.5 min. It obtained a high eco-score of 91 by the “Analytical Eco-Scale” tool. The developed method is eco-friendly and fast, which is suitable for the quality evaluation of Cordyceps and related products.
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Food Additives and Contaminants Part A-Chemistry Analysis Control Exposure & Risk Assessment
·
2021
·
IF 3.057
Shaomin Ma,Xiuyi Jin,Huan Wei,Yue Liu,Ming Guo
In this paper, novel high extraction efficiency hydrophobic eutectic solvents (DESs), n-octanoic acid as a hydrogen bond donor (HBD) and menthol as a hydrogen bond acceptor (HBA), were selected from five hydrophobic DESs to extract trace diphenylamine (DPA) in fruits apple, pear and orange under ultrasonic-assisted liquid-liquid micro-extraction (UA-LLME) technology before high-performance liquid chromatography (HPLC) analysis. Working parameters such as the DESs type, molar ratio, extractant volume, and ultrasonic time of the LLME hydrophobic DESs technology were optimised. Average recoveries between 96% and 108% were obtained on actual samples. This method gave lower detection limit (LOD) than other existing methods due to combining the high-efficiency extraction of hydrophobic DES and high sensitivity of fluorescence detector. This method was sensitive and eco-friendly, and can be used for the determination of trace components in fruits.
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JOURNAL OF FOOD SCIENCE
·
2021
·Vol. 86
·期 11
·4828-4839
·
IF 3.167
Jing-wen Hao,An-ling Zhu,Nai-Dong Chen,Xiao-quan Liu,Qiang Li,Hui-min Xu,Wei-Han Yang,Chao-feng Qin,Jin-Dong Wu
A phenylhexyl isothiocyanate (PITC) precolumn derivatization quantitative analysis of multicomponents by a single marker (QAMS) strategy for the simultaneous analysis of 20 free amino acids (FAA) in Dendrobium huoshanense is proposed. The method was validated by the linearity, limit of detection (LDO), and limit of quantitation (LOQ), recovery, precision, and stability. The results showed that when applying the established method, the LOQ of the FFAs was lower than 1 ng/ml except threonine (1.32 ng) and cysteine (1.16 ng). The QAMS investigation revealed that, using any one of the 20 FAAs as the reference internal standard, no significant differences were observed between the external standard method and the QAMS method for the quantification of FAAs in D. huoshanense by PITC precolumn derivatization [The relative standard deviation (RSD, %) by QAMS and ESM were all below 5%]. HPLC fingerprint investigation combined with similar analysis (the similarity values for S1–S25 were >0.875) and quality fluctuation analysis showed that the cultivation environment might have a great effect on the accumulation of FAAs in D. huoshanense . Overall, our study showed that we might increase the accuracy and scope of the simultaneous quantification of multicomponents using the QAMS technique by being derivatized with a strong UV absorbing group, and QAMS combined with chromatographic fingerprinting can be considered good quality criteria for the quality control of D. huoshanense and may provide analytical technical support for research on Maillard Reaction during the further processing of D. huoshanense .
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MOLECULES
·
2021
·Vol. 26
·期 11
·3344
·
IF 4.412
Shunyu Yao,Zixi Zhao,Wang Lu,Xin Dong,Jiye Hu,Xiaolu Liu
The chemical fungicide fludioxonil is widely used to control post-harvest fungal disease in cherries. This study was implemented to investigate the dissipation behaviours and residues of fludioxonil on cherries. A reliable and efficient analytical method was established. Cherry samples from four product areas were analyzed by QuEChERS and HPLC-MS/MS methods with acceptable linearity (R2> 0.99), accuracy (recoveries of 81–94%), and precision (relative standard deviation of 2.5–11.9%). The limits of quantification (LOQs) and limits of detection (LODs) of cherries were 0.01 mg/kg and 0.005 mg/kg. The dissipation of fludioxonil on cherries followed first order kinetics with half-lives of 33.7–44.7 days. The terminal residues of fludioxonil were all lower than 5.00 mg/kg, which is the MRL recommended by the European Commission. According to Chinese dietary patterns and terminal residue distributions, the risk quotient (RQs) of fludioxonil was 0.61%, revealing that the evaluated cherries exhibited an acceptably low dietary risk to consumers.Keywords:fludioxonil;cherry;HPLC-MS/MS;dissipation behaviour;residues;dietary risk assessment
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FOOD CHEMISTRY
·
2020
·
IF 6.306
Shuying Han,Yilin Song,Jiachun Hu,Rui Liu,Yumei Chi,An Kang,Haishan Deng,Dong Zhu
An on-line enrichment-liquid chromatography-fluorescence detection (LC-FD) method was developed for simultaneous determination of nine bisphenols (BPs). In this process, we predicted the separation based on an in-house developed software allowing for calculating both retention time ( t R ) and half-peak width ( W 1/2 ) of the solute by mobile phase fraction ( φ ) under gradient conditions. The proposed strategy was applied to separation prediction of BPs with high accuracy. Under the optimized conditions, good linearity was obtained with the correlation coefficients ( R 2 ) ranging from 0.998 to 1.000. The recoveries in spiked samples were 91.3–110.7% with the intra-day and inter-day relative standard deviation ranging 0.4–9.6% and 0.5–10.2%, respectively. The limits of detection and quantification were 0.13–66.7 ng L −1 and 0.40–200 ng L −1 . The developed approach was used to monitor the nine BPs in 28 children’s water bottles. The developed method provides an effective way for monitoring bisphenols in other similar matrix.
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FOOD CHEMISTRY
·
2020
·
IF 6.306
Qiuhua Wu,Yuhong Song,Qianqian Wang,Weihua Liu,Lin Hao,Zhi Wang,Chun Wang
A magnetic o -hydroxyazobenzene (M-HAzo) porous organic polymer was facilely prepared by a green azo coupling reaction in aqueous solution. The prepared M-HAzo was applied as a new adsorbent for the first time to pre-concentrate phthalate esters (PAEs) from plastic bottled juice, followed by their determination with high performance liquid chromatography-ultraviolet detection. The effects of various parameters, i.e., the mass ratio of the Fe 3 O 4 @SiO 2 to HAzo, extraction time, ionic strength, pH of the sample, desorption conditions were optimized. Under the optimized conditions, the M-HAzo based method exhibited good performance in terms of linear range (0.3–50.0 μg L −1 ), detection limit (0.08–0.50 μg L −1 ), accuracy (recovery of 78.0–115.0%) and repeatability (relative standard deviation of 2.9–7.8%). This work provides a sensitive method for analysis of PAEs at trace levels in drinks, which is featured with high sensitivity, simple operation and environmentally-friendly merit and will have a promising potential in analysis of other organic pollutants.
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FOOD CHEMISTRY
·
2021
·
IF 7.514
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%.
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