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ANALYTICAL CHEMISTRY · 2015 · IF 5.636

Ultrasensitive and Highly Selective Detection of Bioaccumulation of Methyl-Mercury in Fish Samples via Ag0/Hg0 Amalgamation

Li Deng,Yan Li,Xiuping Yan,Jun Xiao,Cheng Ma,Jing Zheng,Shaojun Liu,Ronghua Yang

Methylmercury (CH3Hg+), the common organic source of mercury, is well-known as one of the most toxic compounds that is more toxic than inorganic or elemental mercury. In seabeds, the deposited Hg2+ ions are converted into CH3Hg+ by bacteria, where they are subsequently consumed and bioaccumulated in the tissue of fish, and finally, to enter the human diet, causing severe health problems. Therefore, sensitive and selective detection of bioaccumulation of CH3Hg+ in fish samples is desirable. However, selective assay of CH3Hg+ in the mercury-containing samples has been seriously hampered by the difficulty to distinguish CH3Hg+ from ionic mercury. We report here that metal amalgamation, a natural phenomenon occurring between mercury atoms and certain metal atoms, combining with DNA-protected silver nanoparticles, can be used to detect CH3Hg+ with high sensitivity and superior selectivity over Hg2+ and other heavy metals. In our proposed approach, discrimination between CH3Hg+ and Hg2+ ions was realized by forming Ag/Hg amalgam with a CH3Hg+-specific scaffold. We have found that Ag/Hg amalgam can be formed on a CH3Hg+-specific DNA template between silver atoms and mercury atoms but cannot between silver atoms and CH3Hg+. With a dye-labeled DNA strand, the sensor can detect CH3Hg+ down to the picomolar level, which is >125-fold sensitive over Hg2+. Moreover, the presence of 50-fold Hg2+ and 106-fold other metal ions do not interfere with the CH3Hg+ detection. The results shown herein have important implications for the fast, easy, and selective detection and monitoring of CH3Hg+ in environmental and biological samples.

CAS / MDL: 115-09-3
研究领域: 环境科学 · 分析化学 · 毒理学
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MICROCHIMICA ACTA · 2015 ·Vol. 182 ·期 9 ·1791-1796 · IF 3.741

Molecularly imprinted polymers for extraction of malachite green from fish samples prior to its determination by HPLC

Li Lu,Lin Zheng-zhong,Chen Xiao-mei,Zhang Hong-yuan,Lin Yi-dong,Lai Zhu-zhi,Huang Zhi-yong

Molecularly imprinted polymer (MIP) particles for malachite green (MG) were prepared by emulsion polymerization using methacrylic acid as the functional monomer, ethylene glycol dimethacrylate as the cross-linker, and a combination of Span-80 and Tween-80 as an emulsifier. The MIP particles were characterized by SEM micrographs and FT-IR spectra. Their binding capacity for MG was evaluated based on kinetic and isothermal adsorption experiments and compared to non-imprinted polymer particles. Analytical figures of merit include an adsorption equilibrium time of 15 min, an adsorption capacity of 1.9 mg∙g‾ 1 in acetonitrile-water (20:80), and an imprinting factor of 1.85. The MIP particles were successfully applied to the extraction of MG from fish samples spiked with MG and the other interfering substances prior to its determination of MG by HPLC. Spiked samples gave recoveries of MG that ranged from 86 to 104 %, much higher than that of the other interfering substance. Molecularly imprinted polymer particles for malachite green (MG) were prepared by emulsion polymerization. They show adsorption capacity of 1.9 mg∙g‾¹ with imprinting factor of 1.85, and were successfully applied to the extraction of MG from spiked fish samples.

研究领域: 分析化学 · 环境科学
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FOOD CHEMISTRY · 2025 · IF 9.8

Development of a semi-automated one-step purification method for determination of 63 pesticides in fish samples by HPLC-MS/MS using natural loofah sponge as a novel adsorbent

Yupeng Wen,Wendi Huo,Xinyuan Zhang,Yingchun Mu,Huan Liu,Chaoying Zhang,Lu Qiao,Jincheng Li

In this study, we developed a miniaturized semi-automatic purification method based on pressure-filtration purification for sensitive HPLC-MS/MS monitoring of pesticides in aquatic products. For the first time, loofah sponge was demonstrated and utilized as a novel green, low-cost, and effective one-step purification adsorbent for fish sample. The developed method consisted of two main steps: first, target analytes were extracted from fish samples using an acetonitrile-based QuEChERS extraction method. Subsequently, the extract was automatically purified through a pressure-filtration purification column in a centrifuge, followed by HPLC-MS/MS analysis. Under optimized experimental conditions, the method exhibited excellent linearity, with a range of 1.0 to 50.0 μg/kg and a correlation coefficient > 0.99. The detection and quantification limits were 0.5 and 1–2 μg/kg, respectively. Recoveries at spiked levels of 2.0, 5.0 and 30.0 μg/kg ranged from 69.95 to 104.88 %, with intra-day RSDs ranging from 0.58 to 15.01 % and inter-day RSDs ranging from 0.72 % to 14.32 %.

CAS / MDL: 631-61-8 64-19-7 64-18-6
研究领域: 食品科学 · 环境科学 · 分析化学
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FOOD CHEMISTRY · 2020 · IF 6.306

Histamine detection in fish samples based on indirect competitive ELISA method using iron-cobalt co-doped carbon dots labeled histamine antibody

Yi-Fang Li,Zheng-Zhong Lin,Cheng-Yi Hong,Zhi-Yong Huang

Due to complex matrixes and specific reagent deficiency, the rapid detection of histamine is still a challenge to date. Based on the high peroxidase-like activity of iron-cobalt co-doped carbon dots, an indirect competitive enzyme-linked immunosorbent assay (ic-ELISA) was established for histamine detection using the mimic enzyme labeled with histamine antibody (His-Ab). Through the competitive binding of the labeled His-Ab to solid-phase and sample antigens, histamine content was detected with a linear range of 2.5–150 μg mL −1 . The detection limit based on 3σ/K was 0.50 mg kg −1 , which was much lower than those of commercial His-kit and HPLC methods. The ic-ELISA method was applied to histamine detection in fish samples with the recovery of (103.4 ± 0.5)%, which was in accord with those of commercial His-kit and HPLC methods. The results indicated that the established ic-ELISA method was suitable for rapid detection of histamine in fish samples with high accuracy, sensitivity and stability.

研究领域: 食品科学 · 免疫学 · 分析化学
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MICROCHEMICAL JOURNAL · 2017 · IF 3.034

Determination of 4-n-octylphenol, 4-n-nonylphenol and bisphenol A in fish samples from lake and rivers within Hunan Province, China

Li Luo,Yuan Yang,Qiang Wang,Hai-pu Li,Zhou-fei Luo,Zhi-peng Qu,Zhao-guang Yang

The presence of endocrine disrupting chemicals such as 4- n -octylphenol, 4- n -nonylphenol and bisphenol A in environmental samples and artificial products may cause health problems for human and organisms. This developed method was efficient for monitoring of those tracing emerging contaminates and the Plackett-Burman factorial design introduced in extraction step was timesaving. Matrix effect was also considered to ensure proper quantitation. Good linearity (r 2   >   0.99), low Method Detection Limits (MDL) and Method Quantitation Limits (MQL) range from 0.18 to 0.54   ng/g and 0.60 to 1.80   ng/g were obtained. Three level spiking experiment (4, 10, 15   ng/g) showed recoveries range from 74% to 113% for 4- n -octylphenol and 4- n -nonylphenol with RSD range from 2% to 11%. The method was finally applied to the analysis of real fish samples taken from Hunan Province, China, offering a reliable and effective means for monitoring of trace emerging contaminates in fishes largely consumed by residents.

研究领域: 环境科学 · 分析化学 · 毒理学
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2019 · IF 2.813

Novel coordination imprinted polymer monolithic column applied to the solid-phase extraction of flumequine from fish samples

Haiyun Zhai,Guohuan Liang,Xiaojing Guo,Zuanguang Chen,Jiaer Yu,Haidan Lin,Qing Zhou

In this study, a coordination imprinted polymer (CIP) solid-phase extraction (SPE) method was developed to determine the residues of flumequine (FLU) in fish samples. Silanized graphene oxide-doped CIP (SGO-CIP) monolithic column was prepared using FLU-Zn 2+ as template in the presence of SGO. The synthesis conditions of SGO-CIP column were optimized by the response surface methodology. Under the optimum conditions, this column showed high specificity to FLU, and the adsorption capacity reached 61.74 ng mg −1 . The enrichment factor of the monolithic column was over 40-fold. Various factors affecting the extraction efficiency of SGO-CIP column during SPE were tested to achieve optimal enrichment and to reduce non-specific adsorption. FLU in fish was detected by using a high-performance liquid chromatography-fluorescence detection system. The detection limit was as low as 0.32 ng g −1 and the recovery was as high as 95.2%, with relative standard deviations of below 5.9%. This simple and sensitive method may be applicable to the determination of FLU residues in foods.

研究领域: 分析化学 · 食品安全 · 环境科学
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JOURNAL OF FOOD COMPOSITION AND ANALYSIS · 2022 · IF 4.52

Development and evaluation of a semi-automatic single-step clean-up apparatus for rapid analysis of 18 antibiotics in fish samples

Shuhe Mu,Tengwang Teng,Ruidong Zhou,Huan Liu,Huiwu Sun,Jincheng Li

Here we report a novel semi-automatic pre-treatment apparatus to fulfill a single-step clean-up aim for rapid quantification of 18 antibiotics in fish samples. Trimethoprim and 17 sulfonamides were extracted from fish samples by acetonitrile solution based on ultrasonic-assisted extraction. Cheap analytical filtration syringe (CAFS) clean-up column was used to fulfill single-step clean-up of the extract which was set on the developed semi-automatic clean-up apparatus. This semi-automatic clean-up apparatus is quite convenient for single-step purification by precisely controlling the flow rate of the extracts, in which up to 10 samples can be purified in parallel at one time. The time needed to clean sample was only about 2 min per 10 samples. Type of compatible purification column ranged from 1 mL (inner diameter × length, 5.6 × 55 mm) to 12 mL (inner diameter × length, 15.6 × 83 mm). The apparatus also did not need additional gas source such as nitrogen or air. After purification, the analytes were simultaneously separated and quantified by high-performance liquid chromatography/quadrupole-linear ion trap tandem mass spectrometry (HPLC-QTRAP-MS/MS). The limits of detections ranged from 0.5 to 1.0 μg kg −1 , and the limits of quantifications ranged from 1.0 to 5.0 μg kg −1 . All the recoveries ranged from 81.39% to 116.01%. Intra-day and inter-day relative standard deviations (RSDs) were lower than 14% for all analytes.

研究领域: 分析化学 · 食品安全 · 环境科学
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BIOSENSORS & BIOELECTRONICS · 2016 · IF 7.476

Fabricating photoelectrochemical aptasensor for selectively monitoring microcystin-LR residues in fish based on visible light-responsive BiOBr nanoflakes/N-doped graphene photoelectrode

Xiaojiao Du,Ding Jiang,Liming Dai,Lei Zhou,Nan Hao,Jing Qian,Baijing Qiu,Kun Wang

The presence of microcystins in fish has been augmenting the risk of toxicity to animal and human health. Herein, a selective and sensitive method for detecting microcystin-LR (MC-LR) in fish samples by integrating the photoelectrochemical (PEC) technique and the specific recognition ability of aptamer was developed. Specifically, as an efficient PEC transducer, the BiOBr nanoflakes/N-doped graphene p–n heterojunction electrode was utilized as the aptamer immobilization platform via the π–π stacking interaction, which would be a biosensor enabling the convenient and exquisite PEC analysis. Subsequently, the PEC response of constructed aptasensor was specific binding to MC-LR. Other isoforms did not interfere with the detection process, and thus, it could be applied for the highly selective determination of MC-LR level. Under the optimized condition, the PEC signal versus the logarithm of the MC-LR concentration was in good linear relationship ranging from 0.1   pM to 100   nM with detection limit about 0.03   pM. The constructed method was employed to analyze fish samples collected from the local supermarket. The overall analytical recovery of MC-LR in the fish matrices ranged from 97.8 to 101.6%, with relative standard deviation (RSD) of 2.52–5.14%, implying it would have great potential in farm product analysis.

CAS / MDL: 6381-92-6 77-86-1
研究领域: 环境科学 · 分析化学 · 毒理学
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JOURNAL OF CHROMATOGRAPHY A · 2014 · IF 4.258

Novel dummy molecularly imprinted polymers for matrix solid-phase dispersion extraction of eight fluoroquinolones from fish samples

Xiaoli Sun,Jincheng Wang,Yun Li,Jiajia Yang,Jing Jin,Syed Mazhar Shah,Jiping Chen

A series of novel dummy molecularly imprinted polymers (DMIPs) were prepared as highly class-selective sorbents for fluoroquinolones. A non-poisonous dummy template, daidzein, was used for the first time to create specific molecular recognition sites for fluoroquinolones in the synthesized polymers. The influence of porogen polarity on dummy molecular imprinting effect was studied. The DMIP prepared using dimethylsulfoxide−acetonitrile (1:1.8, v/v) as porogen achieved the highest imprinting factors (IF) for fluoroquinolones over a range of IF 13.4–84.0. This DMIP was then used for selective extraction of eight fluoroquinolones (fleroxacin, ofloxacin, norfloxacin, pefloxacin, ciprofloxacin, lomefloxacin, enrofloxacin and gatifloxacin) from fish samples based on dummy molecularly imprinted matrix solid-phase dispersion (DMI-MSPD). The extracted fluoroquinolones were subsequently analyzed by high-performance liquid chromatography (HPLC) equipped with a fluorescence detector (FLD). The developed method had acceptable recoveries (64.4−102.7%) and precision (RSDs: 1.7−8.5%, n   =   5) for determination of fluoroquinolones in fish samples fortified at levels of 10 and 100   ng   g −1 . The limits of detection (LODs) for identification of eight fluoroquinolones ranged between 0.06 and 0.22   ng   g −1 . The results demonstrated great potential of the optimized method for sample preparation in routine analysis of trace fluoroquinolones in fish samples.

研究领域: 分析化学 · 食品科学 · 环境科学
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INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES · 2023 · IF 8.2

Development of seaweed-derived polysaccharide/cellulose nanocrystal-based antifogging labels loaded with alizarin for monitoring aquatic products' freshness

Huan Li,Fan Jiang,Jian Chen,Yanbo Wang,Zhigang Zhou,Renjie Lian

Intelligent freshness indicator labels have attracted great interest for their massive potential in monitoring the freshness of aquatic products over the years. However, there is still a challenge where fogging on the labels during dramatic temperature changes affects the reading of freshness. At the same time, the freshness indicator labels need high mechanical strength to resist collision damage during transportation and storage. Herein, an antifogging freshness indicator label was developed based on seaweed extracts and alizarin. Firstly, soluble polysaccharides and insoluble components were extracted from Gelidium amansii , and cellulose nanocrystal (CNC) was further prepared from the insoluble components by sulfuric acid hydrolysis . Subsequently, a polysaccharide-based film was fabricated using soluble polysaccharides as the matrix materials and CNC as the reinforcement agent. Antifogging experiments showed that the hydrophilic composite films presented good antifogging performance. After loading with alizarin, the composite indicator label exhibited both antifogging and freshness-indicating properties for the salmon sample. The work provided a new idea for developing freshness indicator labels suitable for low-temperature transportation and storage.

研究领域: 食品科学 · 材料科学 · 海洋生物学
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MICROCHEMICAL JOURNAL · 2024 · IF 4.9

Development of a monoclonal antibody-based indirect competitive chemiluminescence immunoassay for nitrofurantoin metabolite AHD residue in fish samples

Ruimin Lu,Yan Zhang,Daoping Zeng,Qihua Xu,Dan Wang,Peng Dai,Weijie Deng,Lin Kang,Xiaoxiao Ke,Luying Duan,Yanping Hong,Wuying Yang

An ultrasensitive indirect competitive chemiluminescence immunoassay (icCLEIA) based on monoclonal antibodies (mAb) for the effective detection of nitrofurantoin metabolite 1-aminohydantoin was developed under optimal conditions in our study. 1-aminohydantoin (AHD) was derivatized with m-formylphenoxyacetic acid (MCEP) to obtain a hapten MCEPAHD. The developed icCLEIA based on anti-MCEPAHD mAb showed high sensitivity to competing drugs 2-nitrophenyl derivative of AHD (2NPAHD) with a limit of detection (LOD) 0.04 ng/mL and a 50 % inhibitory concentration (IC 50 ) 0.27 ng/mL, and the icCLEIA had an ultra-high specificity for 2NPAHD, with little cross-reactivity with structural analogues other than parent drug nitrofurantoin. The mean recovery of AHD in fish samples was found to be 97.0 % to 118.5 %, with a coefficient of variation of less than 7.0 %. A comparison of the results of ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with those of icCLEIA demonstrated good linearity. These assay results indicated that the prepared mAb against MCEPAHD and the developed icCLEIA in our research can be used for simple, fast and sensitive detection of AHD residues in animal tissues.

研究领域: 分析化学 · 免疫学 · 兽医学 · 食品安全
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FOOD CHEMISTRY · 2023 · IF 8.8

Hydroxyl and carboxyl group functionalized conjugated microporous nanomaterial as adsorbent for the solid-phase extraction of phenolic endocrine disrupting chemicals from freshwater fish samples

Xiaohuan Zang,Qingyun Chang,Fangyuan Hou,Shuaihua Zhang,Chun Wang,Zhi Wang,Jianzhong Xu

Endocrine disruption chemicals (EDCs) in food can seriously harm human health. In this study, a hydroxyl and carboxyl group functionalized conjugated microporous nanomaterial (CMP) was prepared by Friedel-Crafts reaction and used as solid-phase extraction (SPE) adsorbent. A functionalized CMP based SPE combined with high performance liquid chromatography-diode array detection was built for the determination of phenolic EDCs from nine fish samples. The extraction conditions were optimized by both single factor and response surface methodology (Box-Behnken Design). The established method performed well in terms of the response linearity (in the range of 0.50–100 ng g −1 with coefficient of determination larger than 0.9942), limits of detection (0.15–0.30 ng g −1 , S/N of 3), limits of quantification (0.50–1.00 ng g −1 , S/N = 10), method recoveries (78.4–121 %) and repeatability (relative standard deviation < 11 %). It can be used as an efficient method to detect trace phenolic EDCs in real fish samples.

研究领域: 环境科学 · 分析化学 · 食品安全
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