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JOURNAL OF FOOD SCIENCE · 2019 ·Vol. 84 ·期 5 ·1138-1144 · IF 2.081

Developing and Validating a UPLC-MS Method with a StageTip-Based Extraction for the Biogenic Amines Analysis in Fish

Jingbo Zhang,Jing Hu,Shuai Wang,Xinping Lin,Huipeng Liang,Shengjie Li,Chenxu Yu,Xiuping Dong,Chaofan Ji

To effectively extract biogenic amines (BAs) from complex food matrices is an important issue. In this study, a stop-and-go-extraction tip (StageTip)-based method for simultaneous enrichment of six BAs including histamine, tyramine, putrescine, cadaverine, tryptamine, and β-phenylethylamine in fish samples was developed and optimized. This StageTip-based BAs extraction method required short extraction time, small sample size, and minimal consumption of organic solvents. In addition, an ultrahigh-performance liquid chromatography coupled with triple quadrupole mass spectrometer was used to identify and quantify BAs without derivatization. Target recovery efficiencies of BAs from spiked fish samples ranged from 84% to 110%. Linear regression models were established to determine BAs in the range of 0.4 to 3.0 mg/L ( R 2 > 0.995). Good repeatability was obtained with relative standard deviation of peak areas (1.17 to 5.61%) and retention time (0.09 to 0.20%). High sensitivity was achieved for the detection of six BAs (0.064 to 1.00 ng/L for the limit of detection, 0.10 to 5 ng/L for the limit of quantification). The proposed method had an obvious advantage in the analysis of BAs in complex food matrices such as fish tissues since it could reflect the subtle distribution of BAs from one fish fillet. Practical Application A StageTip-based BAs enrichment combined with UPLC-MS analysis method was developed and optimized, which was low - cost , environmentally friendly, and with good analytical performances. As such, it has the potential to become a powerful tool for the analysis of BAs in different complex food matrices.

研究领域: 食品科学 · 分析化学
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MICROCHIMICA ACTA · 2017 ·Vol. 184 ·期 7 ·2249-2254 · IF 4.58

Visual and photometric determination of histamine using unmodified gold nanoparticles

Huang Conghui,Wang Shuzhan,Zhao Wenfeng,Zong Chenghua,Liang Aiye,Zhang Qingquan,Liu Xiaojun

The authors describe a colorimetric approach for on-site monitoring of histamine based on the use of gold nanoparticles (AuNPs) that have a negatively charged surface due to the presence of adsorbed citrate ions. Histamine has two basic functional groups, an aliphatic amino group and an imidazole ring. Under the experimental conditions, the protonated aliphatic amino group drives the imidazole ring into close proximity to the AuNPs due to electrostatic attraction. This accelerates the replacement of citrate ions by the imidazole ring because of the strong affinity between imidazole and AuNPs. As a consequence, the two groups synergistically induce the aggregation of the AuNPs and trigger a visible color change from red to blue. The minimum visually detectable histamine concentration is 1.81 μM, which is comparable to the limit of detection (LOD) of the electrochemical approaches at a signal-to-noise ratio of 3:1. When using absorbance at 522 nm, the LOD is lowered to 38 nM. The method was applied to the determination of histamine in fish samples. Schematic of the detection scheme: Histamine induces gold nanoparticle aggregation and triggers a visible color change. The minimum visually detectable histamine concentration by bare eye is 1.81 μM. When using absorbance at 522 nm, the LOD is lowered to 38 nM.

研究领域: 分析化学 · 食品科学
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Food Chemistry-X · 2023 · IF 6.1

Novel filter-press single-step cleanup approach facilitated rapid screening and accurate quantification of 112 veterinary drugs in aquatic products

Jincheng Li,Ruidong Zhou,Guangxin Yang,Essy Kouadio Fodjo,Tengwang Feng,Huiwu Sun,Dongmei Huang,Cong Kong,Huan Liu

In this study, a novel filter-press cleanup column was developed as a single-step cleanup approach for the rapid screening and quantification of 112 veterinary drugs in fish samples. Fish muscle samples were extracted with acetonitrile and ethyl acetate, sequentially. After concentration and reconstitution, N -propylethylenediamine (PSA) sorbent, packed in filter-press column, allows rapid single-step cleanup operation, while UHPLC-Q-Orbitrap-HRMS provides high-precision mass information in multi-residue screening. Under optimum settings, the detection and quantification limits were validated at 0.5 and 2.0 μg·kg −1 , for all analytes, respectively. The ranges of recoveries were from 35.3 to 138.4%. Most of these target analytes (82%) could be measured with recoveries between 60 and 130%, and intra-day RSDs ranging from 1.9 to 26.1%. This method was further applied to evaluate the residual of veterinary drugs in fish samples from four cities in China, and results demonstrated its practicability for multi-residue monitoring veterinary residues for food safety administration.

CAS / MDL: 64-18-6
研究领域: 分析化学 · 食品科学 · 环境科学
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FOOD CHEMISTRY · 2017 · IF 4.529

Speciation analysis of six arsenic species in marketed shellfish: Extraction optimization and health risk assessment

Yuyu Jia,Lin Wang,Li Ma,Zhaoguang Yang

A comparative study between microwave assisted and sonication methods was carried out to extract arsenic (As) species in shellfish samples using different extractants. Six As species including arsenite [As(III)], arsenate [As(V)], monomethylarsonic acid (MMA), dimethylarsinic acid (DMA), arsenobetaine (AsB) and arsenocholine (AsC) were simultaneously separated and determined by the HPLC–ICP-MS method. The microwave assisted method exhibited higher efficiency than sonication, especially using diluted HNO 3 as extractant. By compromising extraction efficiency, pretreatment time and stability of As species, the microwave assisted method using 1% HNO 3 at 100   °C for 1.5   h was selected to extract As from real samples. The proposed method has been applied to extract and determine As species in shellfish samples. The result of correlation analysis indicated that the proportion of AsB in the shellfish samples was decreased with total As concentration increasing due to the biotransformation threshold from inorganic As to AsB.

研究领域: 环境科学 · 分析化学 · 食品安全
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY · 2022 ·Vol. 415 ·期 18 ·4265-4275 · IF 4.478

PEG-modified halloysite as a hydrophilic interaction and cation exchange mixed-mode sorbent for solid-phase extraction of biogenic amines in fish samples

Wang Tingting,Chen Yihui,Hou Chunyan,Qiao Xiaoqiang

A novel type of PEG-modified halloysite was prepared and used as a hydrophilic interaction and cation exchange mixed-mode sorbent for solid-phase extraction of biogenic amines in fish samples. The eluates were analyzed by high-performance liquid chromatography-ultraviolet detection after the derivatization with benzoyl chloride. The developed sorbent was characterized by scanning electron microscopy, infrared spectroscopy, X-ray diffraction, zeta potential analyzer, and thermo-gravimetric analysis. After the optimization of various parameters influencing the extraction efficiency, the PEG-modified halloysite-based SPE method was evaluated. The adsorption capacities of putrescine, spermine, phenethylamine, and histamine were as high as 9.3, 8.5, 5.7, and 5.6 mg g −1 , respectively. Satisfactory reproducibility of sorbent preparation was obtained with within-batch and batch-to-batch relative standard deviations (RSDs) lower than 3.9% and 8.6%, respectively. The biogenic amine spiking recoveries in fish samples ranged from 84.3 to 105.5% with good RSDs lower than 7.8%. Intra-day and inter-day precision, expressed as RSDs, were better than 8.8%. The limits of detection of histamine, putrescine, phenethylamine, and spermine were 9.4, 1.9, 0.5, and 0.9 μg L −1 , respectively. This work provides a new hydrophilic interaction and cation exchange mixed-mode sorbent and is successfully applied to the extraction of trace biogenic amines from fish samples. Graphical Abstract

研究领域: 分析化学 · 食品科学
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2018 · IF 2.441

Determination of semicarbazide in fish by molecularly imprinted stir bar sorptive extraction coupled with high performance liquid chromatography

Tang Tang,Fangdi Wei,Xu Wang,Yujie Ma,Yueyue Song,Yunsu Ma,Quan Song,Guanhong Xu,Yao Cen,Qin Hu

A novel molecularly imprinted stir bar (MI-SB) for sorptive extraction of semicarbazide (SEM) was prepared in present paper. The coating of the stir bar was characterized by scanning electron microscopy, Fourier-transform infrared spectroscopy, dynamic adsorption and static adsorption tests. The saturated adsorption of MI-SB was about 4 times over that of non-imprinted stir bar (NI-SB). The selectivity of MI-SB for SEM was much better than NI-SB. A method to determine SEM was established by coupling MI-SB sorptive extraction with HPLC-UV. The liner range was 1–100   ng/mL for SEM with a correlation coefficient of 0.9985. The limit of detection was about 0.59   ng/mL, which was below the minimum required performance limit of SEM in meat products regulated by European Union. The method was applied to the determination of SEM in fish samples with satisfactory results.

研究领域: 分析化学 · 食品安全
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FOOD CONTROL · 2022 · IF 6.652

Surface-enhanced Raman spectroscopy tandem with derivatized thin-layer chromatography for ultra-sensitive on-site detection of histamine from fish

Sihan Zhang,Qinzhen Fan,Jiaqi Guo,Xianhe Jiao,Xianming Kong,Qian Yu

Sensitive and rapid detection of histamine in fish sample was important for human health. A novel and facile method for on-site detecting histamine in fish was developed by tandem surface-enhanced Raman spectroscopy (SERS) with derivatized thin-layer chromatography. Histamine in tuna was firstly separated by TLC process on a diatomite plate, and then derivatized with fluorescamine (FSA). SERS is used for identification of histamine derivative by a portable Raman spectrometer. The operating conditions were optimized for improving the detection performance. Diatomite plate was suitable for separation and derivatization, 40 times concentrated Au colloid, 1 mM of FSA at pH = 8 were appropriate for the derivatization and SERS detection, and the limit of detection of histamine could achieve 9 ppb. The results indicated that the proposed method not only visualized the histamine on TLC plate but also improve the sensitivity in SERS, that could be employed for the on-site separating and detecting histamine from fish sample.

研究领域: 食品科学 · 分析化学
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CHROMATOGRAPHIA · 2021 ·Vol. 84 ·期 9 ·861-868 · IF 2.044

Capillary Electrophoresis-Indirect Laser-Induced Fluorescence Detection of Neomycin in Fish

Huang Yejing,Han Xiufen,Yu Xiao,Wang Shumei,Zhai Haiyun

A capillary electrophoresis-indirect laser-induced fluorescence detection method was established for neomycin detection in fish. With rhodamine 6G as the background fluorescent substance, neomycin with weak ultraviolet absorption can be detected effectively. The types and concentrations of background buffer, pH, and separation voltage which affected the separation and analysis were all studied. With the optimal conditions, the limit of detection of neomycin was 5.0 ng/g, the recovery of fish samples is between 95.2 and 99.7%, and the relative standard deviation is between 2.7 and 3.6%.

研究领域: 分析化学 · 食品科学
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Analytical Methods · 2023 ·Vol. 15 ·期 18 ·2199-2209 · IF 3.1

A ratiometric electrochemical sensor for detecting lead in fish based on the synergy of semi-complementary aptamer pairs and Ag nanowires@zeolitic imidazolate framework-8

Kuiguo Han,Liang Chen,Wen Zhang,Yanqun Tong,Jiyong Shi,Xiaoyu Su,Xiaobo Zou

This work describes the synergistic application of semi-complementary aptamer pairs and signals on–off ratio strategies on glassy carbon electrodes (GCE) for detecting lead ions (Pb2+) in fish. Gold nanoparticles (AuPNs) as the electrode substrate can provide added binding sites for the aptamers and improve the conductivity of the electrodes. Pb2+ aptamers containing ferrocene (Fc) molecules act as molecular recognizers in the sensing system. In the presence of target ions, Fc signals are affected by conformational changes of the aptamer. The “Ag nanowires@zeolitic imidazolate framework-8 with methylene blue (AgNWs@ZIF-8/MB)” can be semi-complementary to the Pb2+ aptamer after binding to single-stranded DNA (S1). However, S1/AgNWs@ZIF-8/MB self-assembled with Pb2+ aptamer (Apt) by hybridization incubation was quickly replaced by Pb2+ competitively, resulting in the loss of methylene blue (MB) signaling molecules. Hence, the internal reference signal (MB) and conformation change signal (Fc) comprise the ratio sensing system well. Morphology, spectroscopy, and electrochemistry methods have validated the modification and sensing behaviors. The used Apt has made considerable progress in analytical performance. In interference studies and stability checks, the ratio measurement signal IFc/IMB is a more reliable signal than the single signal readout. Following a log-linear relationship, this sensor provides a wide linear range. Furthermore, the proposed sensor can be used to determine Pb2+ in fish samples, and the results agree with those obtained using ICP-MS and recovery tests.

研究领域: 生物化学 · 分析化学 · 环境科学
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JOURNAL OF SEPARATION SCIENCE · 2014 ·Vol. 37 ·期 13 ·1591-1600 · IF 2.594

Multi-walled carbon nanotube modified dummy-template magnetic molecularly imprinted microspheres as solid-phase extraction material for the determination of polychlorinated biphenyls in fish

Xiaowen Du,Saichai Lin,Ning Gan,Xidong Chen,Yuting Cao,Tianhua Li,Pan Zhan

Novel multi-walled carbon nanotube modified dummy-template molecularly imprinted microspheres (MWCNTs@DMMIPs) were successfully synthesized as adsorbents for six kinds of polychlorinated biphenyls (PCBs). MWCNTs@DMMIPs were prepared by a surface molecular imprinting technique. Core–shell Fe 3 O 4 @SiO 2 nanoparticles were employed as magnetic support. 3,4-Dichlorobenzene acetic acid was used as a dummy template instead of PCBs, methacrylic acid was used as functional monomer and ethylene glycol dimethacrylate was used as the cross-linker. The resulting absorbent was characterized by various methods. The adsorbent was employed for extracting PCBs and exhibited good selectivity and high adsorption efficiency. Furthermore, it was reusable and capable of magnetic separation. Adsorption kinetics fit well with a pseudo-second-order kinetic equation and also exhibited a three-stage intra-particle diffusion model. The Freundlich model was used to describe the adsorption isotherms. The materials were successfully applied to the magnetic dispersive solid-phase extraction of six kinds of PCBs followed by gas chromatography with mass spectrometry determination in fish samples, the limit of detection of six kinds of PCBs were 0.0028–0.0068 μg/L and spiked recoveries ranged between 73.41 and 114.21%. The prepared adsorbent was expected to be a new material for the removal and recovery of PCBs from contaminated foods.

研究领域: 环境科学 · 分析化学
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SPECTROCHIMICA ACTA PART A-MOLECULAR AND BIOMOLECULAR SPECTROSCOPY · 2017 · IF 2.536

Detection of trace tetracycline in fish via synchronous fluorescence quenching with carbon quantum dots coated with molecularly imprinted silica

Ji Yang,Zheng-Zhong Lin,A-Zha Nur,Yan Lu,Ming-Hui Wu,Jun Zeng,Xiao-Mei Chen,Zhi-Yong Huang

A novel fluorescence-based sensor combining synchronous fluorescence spectroscopy (SFS) with molecularly imprinted polymers (MIPs) was fabricated with reverse microemulsion method. Tetracycline (TC), (3-aminopropyl) triethoxysilane (APTES), tetraethyl orthosilicate (TEOS) and carbon quantum dots (CDs) were used as template, functional monomer , cross-linker and signal sources respectively in the probe preparation. A synchronous fluorescence emission (λ em ) at 355   nm was observed for the prepared MIP-coated CDs (MIP@CDs) particles when the wavelength interval (Δλ) was set as 70   nm, and the synchronous fluorescence intensity could be rapidly and efficiently quenched by TC based on inner filter effect (IFE). The quenching efficiencies of synchronous fluorescence intensity was linearly fitted with tetracycline (TC) concentrations ranging from 0.1 to 50   μmol   L −   1 with a detection limit (DL) of 9   nmol   L −   1 (3 σ , n   =   9). The MIP@CDs was used as a probe to detect TC in fish samples with the recoveries ranging from 98.4% to 103.1% and the relative standard deviation less than 6.0%. The results illustrated that the as-prepared MIP@CDs could be applied to the detection of trace TC in fish samples with rapidity, high sensitivity and accuracy.

研究领域: 分析化学 · 食品安全
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RSC Advances · 2019 ·Vol. 9 ·期 29 ·16831-16838 · IF 3.049

The visual detection of anesthetics in fish based on an inverse opal photonic crystal sensor

Shili Chen,Hui Sun,Zhenjian Huang,Zhenkai Jin,Siyang Fang,Jiahua He,Yangyang Liu,Yi Zhang,Jiaping Lai

A novel smart sensor for the rapid and label-free detection of benzocaine has been developed based on the combination of photonic crystal (PC) and molecular imprinting polymer (MIP) techniques. A molecularly imprinted photonic crystal (MIPC) hydrogel film was prepared via a non-covalent, self-assembly approach with a PC mould. With a highly ordered inverse opal structure, the resulting benzocaine MIPC exhibited high sensitivity, smart specificity, quick response times and good regeneration abilities. It can give rise to a readable optical signal and color change upon binding with benzocaine, with a detection limit of 16.5 μg mL−1. The sensor has been successfully used to visually estimate benzocaine concentrations in fish samples. In comparison with HPLC, the developed MIPC sensor has shown satisfactory accuracy in terms of results. It has great potential for on-site screening and the visual detection of trace benzocaine in real samples.

研究领域: 生物化学 · 传感技术 · 水产科学
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