Food Analytical Methods
·
2018
·Vol. 11
·期 10
·2885-2896
·
IF 2.245
Qi Mengyu,Tu Chunyan,Li Zhaoqian,Wang Weiping,Chen Jianrong,Wang Ai-Jun
A rapid, sensitive, and economical pipette tip solid phase extraction (PT-SPE) based on graphene oxide/polypyrrole (GO/PPy) coupled with high performance liquid chromatography (HPLC) was developed for the extraction and determination of sulfonamides (SAs) in honey and milk samples. The PT-SPE procedure involved only 3.0 mg of adsorbent, 3 min adsorptive extraction time, and less than 1.0 mL of solvent consumption (sample, washing, or eluent). Under the optimal conditions, good linearities (0.01–10.00 μg mL −1 ) were obtained with correlation coefficients ( r ) > 0.9996. The limits of detection ( S / N = 3) were in the range of 1.04–1.50 ng mL −1 . Meanwhile, the proposed method was successfully applied for the analysis of SAs in honey and milk with average recoveries within 62.3–109.0% and relative standard deviations less than 11.2%. The results demonstrated that the developed PT-SPE-HPLC method was suitable for the analysis of SAs in complex matrix due to its high sensitivity and accuracy.
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TALANTA
·
2015
·
IF 3.545
Qiyuan Shi,Jiale Chen,Qinfen Zhou,Houliang Lei,Lianjun Luan,Xuesong Liu,Yongjiang Wu
A rapid and efficient method for the identification of antioxidants in the traditional Chinese medicine Polygalae Radix (PR) by HPLC–ESI-Q-TOF-MS/MS is described. The method is based on the hypothesis that upon reaction of antioxidants with 1,1-diphenyl-2-picrylhydrazyl (DPPH), the peak areas of compounds with potential antioxidant activities in the HPLC chromatogram will be significantly reduced in comparison to the untreated sample. The identity confirmation was achieved by Q-TOF-MS/MS technique. With this method, eight components were proposed possessing potent antioxidant activity. They were identified as sibiricose A5, sibiricose A6, sucrose monoester, polygalaxanthone III, tenuifoliside B, 3',6-disinapoylsucrose (DISS), sucrose diester , tenuifoliside C, respectively. DISS was proposed to be the most potent one. The antioxidant activity of DISS was evaluated by DPPH, ABTS radical scavenging assay and ferric-reducing antioxidant power (FRAP) assay in vitro. Vitamin C (Vc) was used as positive control substance. DISS showed moderate DPPH (DISS's IC 50 value was 1024.17 μg/mL, Vc's was 294.68 μg/mL) and ABTS (IC 50 324.13 μg/mL, Vc's was 117.50 μg/mL) free radical scavenging capacity and ferric-reducing antioxidant power. DISS can be used as a new source of natural antioxidant in foods and cosmetics.
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Food Analytical Methods
·
2013
·Vol. 7
·期 7
·1381-1386
·
IF 1.969
Ma Xiaoxing,Wang Juntao,Wu Qiuhua,Wang Chun,Wang Zhi
A new analytical method by graphene-reinforced hollow fiber liquid-phase microextraction combined with high-performance liquid chromatography fluorescence detection was developed for the determination of bisphenol A and 4- tert -butylphenol in bottled juices. Several important experimental parameters were studied to get optimal extraction conditions for the analytes. Under the optimized conditions, the method showed a good performance having a linear response in the range from 0.05 to 10.0 ng mL −1 with the correlation coefficients ( r ) of 0.9965–0.9994 and limits of detection of 0.01 ng mL −1 . The relative standard deviations were in the range from 6.4 to 7.2 % at the spiked concentration of 1.0 ng mL −1 . The method combines the high-adsorption capacity of graphene and the excellent clean-up performance of hollow fiber liquid-phase microextraction and has been successfully applied to the analysis of the analytes in bottled juice samples.
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Analytical Methods
·
2015
·Vol. 8
·期 5
·1003-1012
·
IF 1.821
Xiaoxiao You,Ligang Chen
A new strategy for the isolation and enrichment of sulfonylurea herbicides in grain samples was obtained by using magnetic molecularly imprinted polymers (MMIPs) using carbon nanotubes as the matrix, nicosulfuron as the template molecule, 3-aminopropyltriethoxysilane as the functional monomer, tetraethyl orthosilicate as the cross-linker and cetyl trimethylammonium bromide as the dispersant. The characteristics of the MMIPs were assessed by transmission electron microscopy, vibrating sample magnetometry, X-ray diffractometry, elemental analysis, the Brunauer–Emmett–Teller method and Fourier transform infrared spectroscopy. The binding characteristics of the imprinted materials were researched using isothermal adsorption experiments, kinetics adsorption experiments and selectivity experiments. The recoveries of four sulfonylurea herbicides were more than 80.0% and the detection limits were 0.0107, 0.0151, 0.0147 and 0.0123 μg g−1, respectively. RSDs of intra-day and inter-day precisions in the range of 0.7–2.4% and 5.3–8.4% were obtained, respectively. The results demonstrate that MMIPs are promising for the preconcentration, purification and analysis of sulfonylurea herbicides in grain samples.
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TALANTA
·
2014
·
IF 3.511
Minqiong Tang,Qing Wang,Ming Jiang,Li Xu,Zhi-Guo Shi,Ting Zhang,Yan Liu
In the present study, magnetic nanoparticles (MNPs) with phenyl functionalized core and a hydrophilic methylcellulose coating were synthesized. The functionalized MNPs showed excellent dispersibility in aqueous solution and they were applied to magnetic solid phase extraction (MSPE) of sildenafil and its metabolite, desmethyl sildenafil, from human urine and plasma samples followed by high performance liquid chromatographic analysis. The factors that may influence the extraction, including the amount of MNPs, pH and salt concentration of sample solution, extraction and desorption time, and the volume of desorption solvent, were investigated in detail. Under the optimum MSPE conditions, the developed method showed satisfactory reproducibility with intra-day and inter-day relative standard deviations less than 8.2% and low limits of detection of 0.41–0.96 ng mL −1 from urine and plasma samples. The proposed material possessed good water compatibility and demonstrated excellent applicability for biological samples.
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Food Analytical Methods
·
2014
·Vol. 8
·期 2
·428-437
·
IF 1.802
Zeng Fang,Ou Jun,Huang Yufen,Li Qian,Xu Guizhi,Liu Zhongzhen,Yang Shaohai
The present paper reports the application of an optimized pre-column derivatization procedure with aminoquinolyl- N -hydroxysuccinimidyl carbamate (AQC) to the determination of 21 free amino acids in fruit juices. The method permitted the optimal separation of 21 amino acids and ammonium in 30 min. Excellent response linearity was obtained from 2 to 1,000 μM for all amino acids, except tryptophan, for which the linearity was 5–1,000 μM. The fluorescence detection limits ranged from 0.08 pmol (phenylalanine) to 0.69 pmol (cysteine), except for tryptophan (7.89 pmol), for a signal-to-noise ratio of 3. The relative standard deviations of peak areas ranged from 0.1 to 0.4 % for intraday analysis and from 2.1 to 5.0 % for interday analysis. The method was applied to analyze the free amino acids in six fruit juices, and the recoveries of the proposed method were 90.4 to 103.3 %. The total free amino acid content ranged from 56.97 mg L −1 (apple) to 469.45 mg L −1 (longan) in six fruit juices. Aspartic acid (Asp), glutamic acid (Glu), asparagine (Asn), serine (Ser), and glutamine (Gln) were present in higher levels in most samples, whereas cysteine (Cys) was below the detection limit in the selected samples. Notable advantages of this method include its speed, ease, low cost, good repeatability, high sensitivity, excellent precision and accuracy, and anti-interference in high-sugar matrices.
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TALANTA
·
2016
·
IF 4.035
Xixi Wang,Xueying Li,Xiaoya Jiang,Peipei Dong,Haiyan Liu,Ligai Bai,Hongyuan Yan
A high performance liquid chromatography (HPLC) monolithic column was prepared by redox polymerization of styrene , dipentaerythritol hexaacrylate (DPHA) and ethylene glycol dimethacrylate (EDMA) in a porogen system of n-propanol/PEG400. The monolith was characterized by scanning electron microscopy (SEM), mercury intrusion porosimetry (MIP) and the results indicated that the monolith had a stable and homogeneous structure. The porosity of the monolithic column was 75.86% and average pore diameter was 2.1 µm. Several alkylbenzenes and anilines were used to evaluate the column performance in terms of hydrophobicity . Then the column was applied to separate small molecules including phytosterol and BSA tryptic digest. Finally, five standard proteins, egg white and plasma were separated respectively and high separation capacity of protein was obtained.
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JOURNAL OF CHROMATOGRAPHY A
·
2016
·
IF 3.926
Xiao-Fei Gu,Yue Zhao,Kan Li,Meng-Xiang Su,Fang Yan,Bo Li,Ying-Xiang Du,Bin Di
Structure elucidation of volatile aromatic isomers at trace level has long been considered as an elusive task, due to their structural similarities and similar polarities, even with the aid of many spectroscopic techniques such as mass spectrometry and nuclear magnetic resonance (NMR) spectroscopy. Single-crystal X-ray diffraction (SCD) is recognized as one of the most powerful structural elucidation techniques. The recently developed crystalline sponge method overcomes the intrinsic limitation of SCD that the target molecules must be single crystals, being able to analyze non-crystalline and trace-amount compounds without any special treatment. In order to investigate whether the crystalline sponge method could be used for the structure elucidation of closely related isomers or other volatile and even oily compounds in complex mixtures at trace level, we combined HPLC separation with the crystalline sponge method for X-ray crystallographic analysis. In this paper, two pairs of volatile aromatic isomers including cis / trans isomers of asarone and positional isomers of carvacrol and thymol, as well as the main volatile component in essential oil extracted from Acorus Tatarinowii , were first isolated by HPLC and encapsulated into the crystalline sponge then elucidated by X-ray crystallographic analysis. Direct observation of these volatile compounds by X-ray crystallography was achieved using only microgram quantities without crystallization or derivatization. Unambiguous identification of these compounds was realized without reference standards. This strategy offers a promising platform capable of providing high-confidence detailed structural information of closely related isomers as well as other volatile and even oily compounds in complex mixtures in microgram quantities.
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ANALYTICAL LETTERS
·
2025
·
IF 1.8
Wanying Zhao,Yanqin Chen,Jun Tan,Yanru Bai,Fudong Ma
A method utilizing high-performance liquid chromatography with evaporative light scattering detection (HPLC-ELSD) has been developed and validated for the simultaneous determination of raffinose, glucose, sucrose, and stachyose in waste liquid from cottonseed processing and in byproducts including cottonseed meal. The separation was performed using a carbohydrate ES column (250 × 4.6 mm, 5 μm) and isocratic elution with acetonitrile and water (70:30, v/v). The temperature of the column oven was maintained at 35 °C. The drift tube temperature for evaporative light scattering detection (ELSD) was operated 40 °C, while the nitrogen flow was set to 1.5 L·min−1. The saccharides were separated by HPLC-ELSD within 20 min. The coefficients of determination (R2 = 0.9986–0.9999) indicate that there was a linear relationship between saccharides and the response. The limits of detection were 0.004–0.023 mg·mL−1 and the quantification range was from 0.013 to 0.080 mg·mL−1. The intraday and interday precision were from 0.05 to 0.55% and 0.20 to 0.58%, respectively. The recovery was from 102.75 ± 2.03% to 106.76 ± 2.09% and the relative standard deviations were 1.87 to 1.98%. The method exhibited good stability in determining four saccharides in cottonseed processing waste liquid and the resultant byproduct cottonseed meal. This method exhibits high separation efficiency and sensitivity, excellent precision, and simplicity, which allows determination of the high value-added product, raffinose, in cottonseed processing waste liquid and meal.
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LWT-FOOD SCIENCE AND TECHNOLOGY
·
2024
·
IF 6
Dan Wei,Qiao Deng,Jianliang Li,Jingjing Xu,Ming Guo,Huizhen Wu,Ju Zhang,Jianchang Jin,Xu Wang
Mycotoxins co-contamination in soybean poses great risks to human health, however, due to their diverse structures, it is difficult to simultaneously extract and detect these multi-mycotoxins. By incorporating modification of hydrophilic carboxyl groups with the hydrophobic properties of covalent organic frameworks, a stable cubic carboxyl-functionalized magnetic amide-linked covalent organic framework were fabricated, characterized and utilized as adsorbents for magnetic solid phase extraction (MSPE) of eleven frequently detected mycotoxins from soybeans followed by HPLC-MS/MS analysis. The key MSPE parameters were screened using the Plackett-Burman design and optimized with the Box-Behnken design for response surface methodologies. Under the optimal experimental conditions, the linear range was 0.2–50 μg/kg, the limits of detection were 0.1–1.4 μg/kg. The established method was applied for the soybean analysis with satisfactory recoveries (70.8–108.3%) and precision (intra- and inter-relative standard deviations of 2.1–9.2% and 1.6–11.1%, respectively). With proper modification, this method may have great application potential for simultaneously analyzing and monitoring the multi-mycotoxin contamination in foods to ensure consumer safety and public health.
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TALANTA
·
2024
·
IF 5.6
Shurong Chen,Min Zhu,Ying Wang,Jinru Ding,Mingji Tan,Jindou Zhao,Jiahan Xie,Zhibing Wang
A novel temperature-responsive supramolecular solvent was prepared with cetyltributylphosphonium tetrafluoroborate and sodium citrate. It served as the extraction solvent of dispersive liquid-liquid microextraction for the extraction and enrichment of pyrethroids in tobacco samples. In this study, the preparation of the temperature-responsive supramolecular solvent and the extraction of the target analytes were integrated into one step, which simplified the experimental process. Due to the low melting point of the prepared supramolecular solvent, the traditional liquid-liquid separation can be converted to solid-liquid separation at low temperatures. This conversion facilitates precise collection of the supramolecular solvent and reduces the loss of target analytes. The composition, structure, physicochemical properties, and micromorphology of the supramolecular solvent were characterized. The formation and extraction mechanism of supramolecular solvent were explored, and the extraction conditions were optimized. The results indicated that good linearity of target analytes ( R 2 > 0.9998) was obtained within the linear range. The limits of detection and quantification for the five pyrethroids were in the range of 0.25–0.50 μg L −1 and 0.85–1.65 μg L −1 , respectively. The present method can be used for the analysis of pyrethroid pesticide residues in tobacco samples.
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JOURNAL OF SEPARATION SCIENCE
·
2017
·Vol. 40
·期 20
·4032-4040
·
IF 2.557
Qingxiang Zhou,Yongyong Yuan,Yalin Wu,Yongli Liu
A novel magnetic core–shell material polyaniline@SiO 2 @Fe (PANI@SiO 2 @Fe) has been successfully synthesized and investigated as an effective adsorbent for the magnetic solid-phase extraction of typical endocrine disrupting compounds such as bisphenol A, tetrabromobisphenol A, and 4-nonylphenol from water samples. The morphology of the as-prepared PANI@SiO 2 @Fe was characterized by transmission electron microscopy and X-ray diffraction. The main parameters that influenced the enrichment performance such as the kind of eluent, amount of adsorbent, volume of eluent, adsorption time, elution time, ionic strength, pH, concentration of humic acid, and sample volume were investigated. Under the optimal conditions, a good linear relationship was found in the range of 0.05–100 μg/L for bisphenol A, 0.05–300 μg/L for tetrabromobisphenol A, and 0.05–250 μg/L for 4-nonylphenol, respectively. The correlation coefficients are all above 0.995. The limits of detection were in the range of 0.009–0.04 μg/L, and precisions were under 3.73% ( n = 6). The real water analysis indicated that the spiked recoveries were in the range of 92.9–98.9% ( n = 3). All these results indicated that the developed method was an efficient tool for the analysis of bisphenol A, tetrabromobisphenol A, and 4-nonylphenol.
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