Analysis of 17β-Estadiol from Sewage in Coastal Marine Environment by Surface Plasmon Resonance Technique

In this study,surface plasmon resonance(SPR)for monitoring 17β-eatradiol(E2)was developed.The small molecule E2 was immobilized on a CM5 sensor chip for an indirect competitive immunoassay to detect E2.The SPR response based on the antigen-antibody reaction was measured by injecting the sample solution into the flow system.The limitation of detection was 0.445 μg/L.The developed SPE-SPR system was applied to analyze the seawater samples.Recovery of E2 was 91.6%-93.1%.Relative standard deviations(RSD)for the E2 assay were between 10.9%-15.1%(n=3).The range of determination of E2 samples from the sewage in the coastal marine environment was between ND(lower than detection limit)and ca.11.78 ng/L.     

L-cysteine modified gold nanoparticles / paper chip system for rapid detection of chiral dopaEI北大核心CSCD

A new detection method for L-Dopa based on paper chips was established. The L-Cys-AuNPs were characterized by their size, zeta potential, and UV-visible absorption spectra. The system had the high selectivity for the colorimetric detection of L-Dopa with the color changing from red to blue. The results were recorded using a common cell phone and subsequently analyzed using Photoshop software. A ratiometric color intensity method was designed for the quantification analysis. The ratio of color intensity at red channel and blue channel (R / B) increases linearly with L-Dopa concentration in the range of 5 to 80 μmol / L (R = 0. 9944), with the limit of detection of 4 μmol / L. The spiked recoveries of samples were 98%-102%. The RSDs of inter-day and intraday were 3. 3% and 3. 8%, respectively. Real samples were detected, and the error between the determination and the labeled value was within 5%. The method can be used to detect L-Dopa in real samples. © 2022, Youke Publishing Co.,Ltd. All rights reserved.     

Determination of silver ion based on the redshift of emission wavelength of quantum dots functionalized with rhodanine

A simple and selective method for the determination of silver ions was developed by utilizing the red- shift in emission wavelength of the core-shell CdSe/Cd5 quantum dots （QDs） functionalized with rhodanine upon the addition of Ag＋. A linear relationship was observed between the shift and the increase in concentration of Ag＋ in the range of 0.0125-12.5 μmol/L. The mechanism of the red-shift was investigated and suggested that the coordination between Ag＋ and rhodanine on the QDs surface caused an increase of particle size, which resulted in the red-shift of the QDs＇ emission wavelength. A detection limit of 2 nmol/L was achieved. The developed method showed superior selectivity and was successfully applied to the determination of silver in environmental samples.     

Electrochemical detection of bisphenol A based on Co nanoparticles/N-doped carbon nanotubes compositesEI北大核心CSCD

Co nanoparticles and nitrogen-doped carbon nanotubes （NCNTs）were prepared by calcination of metal-organic material ZIF-67 in a reductive atmosphere of H2 and Ar gas,and modified on the surface of glassy carbon electrod（GCE）for the detection of bisphenol A（BPA）. The Co/NCNTs composites exhibited superior electrocatalytic performance for BPA oxidation owing to the synergistic effect between chemical composition and the specific structure of the Co/NCNTs composites. In optimal conditions,Co/NCNTs/GCE exhibited a linear range of 0.01-20 μµmol/L for BPA（R2=0.998）. The prepared electrode was employed to detect the content of BPA in real samples with the recoveries of 98.4%-104.6%. © 2023, Youke Publishing Co.,Ltd. All rights reserved.     

Development of an Indirect Competitive ELISA Based on Polyclonal Antibody for the Detection of Diethylstilbestrol in Water Samples

An indirect competitive enzyme-linked immunosorbent assay （icELISA） based on polyclonal antibody for the estrogen diethylstilbestrol （DES） was developed. With this aim, two different haptens mono-O-3-carboxypropyldiethylstilbestrol （DES-CP） and mono-O-carboxymethyldiethylstilbestrol （DES-CM） with carboxylic group that preserve the molecular structure character of diethylstilbestrol were synthesized. The haptens were conjugated with the carder proteins bovine serum albumin （BSA） by mixed-anhydride method for immunogen and conjugated with ovalbumin （OVA） by active ester method for coating antigen. Polyclonal antibodies for diethylstilbestrol were raised by immunizing mice with immune antigen DES-CP-BSA. Under optimized system, the lowest limit of detection （LLD） of diethylstilbestrol was 0.01 ng/mL, and IC50= 1.02 ng/mL. Its analogs were tested and no obvious cross-reactivity was found to anti-diethylstilbestrol antibody. DES-fortified water samples were determined by simple dilution to diminish the matrix effect. The comparison between the amount of DES estimated by ELISA and the amount added indicates good agreement for all water samples tested, with mean recovery values ranging from 86% to 120.2%.     

Analysis of nitrobenzene compounds in water and soil samples by graphene composite-based solid-phase microextraction coupled with gas chromatography–mass spectrometry

In this work, solid-phase microextraction coupled with gas chromatography–mass spectrometry was developed to determine trace levels of nitrobenzene compounds in water and soil samples. Graphene was chosen as the extraction material and its composite was coated on a stainless steel wire through sol–gel technique for the solid phase microextraction. The key parameters influencing the extraction efficiency were optimized. Under the optimal conditions, the linearity for the compounds was observed in the range of 0.02–15.0 mg/L for water samples, and 0.2–60.0 mg/kg for soil samples, with the correlation coefficients（r） of 0.9966–0.9987. The limits of detection of the method were 0.0025–0.005 mg/L for water samples, and 0.02–0.04 mg/kg for soil samples. The recoveries for the spiked samples were in the range of 72.0%–113.2%, and the precision, expressed as the relative standard deviations, was less than 12.1%.     

A new fluorescence probing strategy for the detection of parathion-methyl based on N-doped carbon dots and methyl parathion hydrolase

A new facile fluorescence probing strategy, which was based on N-doped carbon dots(NCDs) and methyl parathion hydrolase(MPH), was developed for the determination of parathion-methyl(PM). The fluorescence intensity of NCDs-MPH system was proportional to PM concentration in the range of 2.38–73.78 mmol/L, with a detection limit of 0.338 mmol/L. Moreover, the present simple and facile method could be used to determine methyl parathion in environmental and agricultural samples successfully.Furthermore, the detection mechanism of this system is inner filter effect and molecular interactions between NCDs and p-nitrophenol, which is the hydrolysis product of PM catalyzed by methyl parathion hydrolase.     

Simultaneous Determination of Epinephrine, Noradrenaline and Dopamine in Human Serum Samples by High Performance Liquid Chromatography with Chemiluminescence Detection

A simple, rapid and accurate high performance liquid chromatographic （HPLC） technique coupled with chemiluminescence （CL） detection was developed for the simultaneous determination of epinephrine （E）, noradrenaline （NA） and dopamine （DA）. It was based on the analyte enhancement effect on the CL reaction between luminol and potassium ferricyanide. The effects of various parameters, such as potassium ferricyanide concentration, luminol concentration, pH value and component of the mobile phase on chromatographic behaviors of the analytes （E, NA and DA） were investigated. The separation was carded out on C18 column using the mobile phase of 0.01 mol/L potassium hydrogen phthalate solution and methanol （92 ： 8, V/V）. Under the optimum condi- tions, E, NA and DA showed good linear relationships in the range of 1 × 10^-8 -5 × 10^-6, 5.0× 10^-9 -1.0× 10^-6 and 5.0×10^-9-1.0× 10^-6 g]mL respectively. The detection limits for E, NA and DA were 4.0×10^-9, 1.0× 10^-9 and 8.0 × 10^-10 g/mL. The proposed method has been applied successfully to the analysis of E, NA and DA in human serum samples.     

ClO3--SO32--Rh6G-SDBS体系的化学发光及其用于亚硫酸根测定

Based on the micelle synergism mechanism, a chemiluminescence （CL） flow system for the determination of sulfite was described. The CL signal generated from the reaction of chlorate with sulfite in acidic solution was very weak, while the interfusion of sodium dodecylbenzenesulfonate （SDBS） resulted in a highly chemiluminescent intensity. The major goal of this work was to investigate and develop the SDBS rnicelle synergetic CL system. The mechanism was proposed and proved by spectrometry. The results indicated that the unique structure of SDBS micelles prorooted the aggregation of rhodamine 6G （Rh6G） and a much easier energy transfer, leading to a marked shift to red in the CL emission. This CL system was developed for the determination of sulfite and the concentration of sulfite was proportional to the CL intensity in the range of 5.0× 10^-8--1.0× 10^-5 mol/L with the detection limit of 1.7×10^-8 mol/L （S/N=3）. The relative standard deviation was 3.3% for 1.0×10^ 6 mol/L sulfite solution with eleven repeated measurements. This method was successfully applied to the determination of sulfite in powder sugar.     

Determination of neomycin in water samples by high performance anion chromatography with pulsed amperometric detection

A simple, fast and reliable method, using high performance anion chromatography with pulsed amperometric detection, had been developed for the analysis of neomycin in water samples. The elution and separation were carried out with an isocratic mobile phase, containing 10 mmol/L NaOH. The influence of the concentration and pH of the mobile phase on the separation and detection was investigated. A quadruple-potential waveform used for the detection was optimized. The detection limit of neomycin was down to 0.027μg/mL. The linearity of neomycin calibration curve ranged from 0.050 to 0.505μg/mL with correlation coefficient of 0.9997. R.S.D. (n = 11) was 4.0%.     

Determination of Pb（II） in environmental water by nano-ceria-graphene modified electrodeEI北大核心CSCD

Nafion solution as a binder,the Gr/CeO2 /Nafion/GCE modified electrode was prepared based on graphene （Gr）-nano cerium oxide （CeO2 ）composite materials. The electrochemical behavior of Pb（II）on the modified electrode was investigated using differential pulse anodic stripping voltammetry （DPASV）. Subsequently,a determination method for Pb（II）was established. The concentrations and ratio of composite materials,buffer solution pH,modification amount,enrichment potential and time were optimized. Under the optimal conditions ,the peak current of Gr/CeO2 /Nafion/GCE showed good linearity in the range of 0.24-48.31 μµmol/L of Pb（II）,and the detection limit was 4.3 nmol/L. Interference experiments showed that the other common anions and cations in water samples caused little interference to Pb（II）detection. Furthermore,the interference of Cu（II）within 10 times is acceptable. The modified electrode was used to the detection of Pb（II） in four complex water samples,and the recovery rates of the spiked assays were from 89.5% to 107.7%. © 2023, Youke Publishing Co.,Ltd. All rights reserved.     

Development of Monoclonal Antibody-based Enzyme-linked Immunosorbent Assay to the Estrogen Diethylstilbestrol

Diethylstilbestrol （DES） is a synthetic estrogen that has ever been used worldwide. Polyclonal antibodies （PAbs） were used in immunoassay for detection of DES residues in environmental and agricultural samples in previous paper. In this paper, an indirect competitive enzyme-linked immunosorbent assay （icELISA） was developed based on monoclonal antibody （MAb） for the determination of diethylstilbestrol. Mono-o-carboxypropyldiethylstilbestrol （DES-CP） and mono-o-carboxymethyldiethylstilbestrol （DES-CME） were synthesized to be haptens. DES-CP was coupled to bovine serum albumin （BSA） to be an immunogen in BALB/c female mouse for MAb production. The MAb was characterized for specificity and affinity to DES in icELISA. Under the optimum condition, the icELISA showed an ICs0 of 9.8 ng/mL, the limit of detection （IC20） of 2.3 ng/mL and a working range of 2-42 ng/mL. Hexestrol and dienestrol exhibited cross-reactivity values were 44% and 27%, respectively. Cross-reactivity of natural estrogen 17β-estradiol was less than 0.1%. The influences of some factors such as salt concentration, pH and organic solvent concentration on the assay were evaluated. The concentrations of DES in the fortified water samples determined by the assay were correlated well with the fortification levels. The results were conf＇m＇ned with analysis by HPLC.     

Osteryoung square wave voltammetric determination of lactose in food samples by a derivative procedure

A method for determination of lactose in food samples by Osteryoung square wave voltammetry （OSWV） was developed. It was based on the nucleophilic addition reaction between lactose and aqua ammonia. The carbonyl group of lactose can be changed into imido group, and this increases the electrochemical activity in reduction and the sensitivity. The optimal condition for the nucleophilic addition reaction was investigated and it was found that in NH4C1-NH3 buffer of pH 10.1, the linear range between the peak current and the concentration of lactose was 0.6-8.4 mg L-l, and the detection limits was 0.44 mg L- 1. The proposed method was applied to the ＇determination of lactose in food samples and satisfactory results were obtained.     

Selection of a DNA aptamer for the development of fluorescent aptasensor for carbaryl detection

An improved ssDNA library immobilized systematic evolution of ligands by enrichment(SELEX) was applied to select aptamers against carbaryl.After nine selection rounds,a highly enriched ssDNA pool was obtained.The Apta3 was demonstrated as the optimal aptame r.In order to facilitate the modification of aptamer,the Apta3 was further truncated with the dissociation constant(K_d) of 0.3 64 ± 0.055 μmol/L and a fluorescent aptasensor was developed.The linear range for carbaryl was from 100 nmol/L to1500 nmol/L,with the limit of detection was as low as 15.23 nmol/L.Besides,the biosensor was validated for the carbaryl spiked real samples,and the recoveries were between 97.7% and 107.3%.     

3DRGO-NiFe2O4/NiO nanoparticles for fast and simple detection of organophosphorus pesticides

The residues of organophosphorus pesticide(OPs)on fruits and vegetables pose a threat to human health,so it is very meaningful to explore simple and fast detect methods for OPs residual.In this work,nickel ferrite/nickel oxide nanoparticles co-loaded three-dimensional reduced graphene oxide(3DRGONiFe2O4/NiO NPs),as a new low cost nanocomposite,was prepared.Based on its high performance mimetic peroxidase activity,a colorimetric method for the detection of OPs has been developed.Dichlorvos was chosen as model compounds to evaluate the detection performance.The detection linear range for dichlorvos is from 50μg/mL to 2.5×10^4μg/mL with a detection limit of 10μg/mL.Furthermore,a test paper can be developed based on the 3 DRGO-NiFe2O4/NiO NPs for visual detection of dichlorvos,and the image information of the paper sensor can be converted into digital signal and quantitative detection by a smartphone.Notably,this method can also be used to detect dichlorvos in real samples,including vegetables and fruits.Thus,the developed naked assay holds great potential in simple,inexpensive and rapid detection of OPs in fruit and vegetable samples.     

强碱阴离子交换树脂及碱性洗脱剂的离子排阻/阴离子交换色谱法同时测定NH4+ ，NO2-和NO3-（英文）

Ion-exclusion/anion-exchange chromatography(IEC/AEC) on a combination of a strongly basic anion-exchange resin in the OH——form with basic eluent has been developed.The separation mechanism is based on the ion-exclusion/penetration effect for cations and the anion-exchange effect for anions to anion-exchange resin phase.This system is useful for simultaneous separation and determination of ammonium ion(NH+4),nitrite ion(NO-2),and nitrate ion(NO-3) in water samples.The resolution of analyte ions can be manipulated by changing the concentration of base in eluent on a polystyrene-divinylbenzene based strongly basic anion-exchange resin column.In this study,several separation columns,which consisted of different particle sizes,different functional groups and different anion-exchange capacities,were compared.As the results,the separation column with the smaller anion-exchange capacity(TSKgel Super IC-Anion) showed well-resolved separation of cations and anions.In the optimization of the basic eluent,lithium hydroxide(LiOH) was used as the eluent and the optimal concentration was concluded to be 2 mmol/L,considering the resolution of analyte ions and the whole retention times.In the optimal conditions,the relative standard deviations of the peak areas and the retention times of NH+4,NO-2,and NO-3 ranged 1.28%-3.57% and 0.54%-1.55%,respectively.The limits of detection at signal-to-noise of 3 were 4.10 μmol/L for NH+4,1.87 μmol/L for NO-2 and 2.83 μmol/L for NO-3.     

Untargeted screening and quantitation of drug residues in bean sprouts by ul⁃tra performance liquid chromatography-quadrupole/orbitrap high resolution mass spectrometryEI北大核心CSCD

A method for the untargeted screening and quantitative analysis of drug residues in bean sprouts by ultra performance liquid chromatography-quadrupole/ orbitrap high resolution mass spectrometry （UPLC-QOrbitrap HRMS） was developed. In the process of screening, the samples were extracted by acetonitrile and the data were gathered via the full MS-ddMS2 mode. In the absence of standards, qualitative analysis was carried out according to the exact mass number of precursor ions and secondary fragment ions information combined with the database. The optimized dispersive solid-phase extraction （d-SPE） method was used to purify the samples. 9 compounds in bean sprouts were screened and quantified on the basis of the peak areas of the precursor ions. 9 compounds showed good linear relationships （R2＞0.990） in the linear concentration ranges. The limits of detection of this method were between 2.0-5.0 μg/kg. The recoveries of 9 compounds at three spiked levels of 5, 10, 50 μg/kg ranged from 80.1% to 111.1%, and the relative standard deviations were less than 15%. © 2023, Youke Publishing Co.,Ltd. All rights reserved.     

Determination of iminodiacetic acid in the glyphosate by ion chromatography

In this paper,a simple method based on ion chromatography（IC） with conductivity detection was developed for the determination of iminodiacetic acid（IDA） in the herbicide of glyphosate.Under optimized chromatographic conditions,good linear relationship,sensitivity and reproducibility were obtained.The detection limit（LOD） for IDA obtained by injecting 25 μL of sample was 31.8 μg/L（S/N = 3）.Relative standard deviation（RSD） of repeated analysis for the peak areas was less than 1.53%（n = 6）.A spiking study was performed with satisfactory recoveries between 92.8%and 103.6%.It was confirmed that this method could be applied in glyphosate products.     

A nonenzyme glucose sensor based on Cu/Ni/CMWCNTs nanocompositesEI北大核心CSCD

Copper-nickel bimetallic nanoparticles decorated on carboxylated multi-walled carbon nanotubes （Cu/Ni/CMWCNTs）were prepared by using a simple one-pot solvothermal method,which was then employed to construct a highly sensitive non-enzymatic glucose sensor. The modified electrode showed high sensitivity and stability in glucose detection,which was mainly attributed to the synergistic effect of the compact copper-nickel nanocomposite and carboxylated multi-walled carbon nanotubes that possessing high specific surface area to increase the number of active sites and to improve the electrocatalytic activity of the modified electrode. The phase structure and morphology of the material were characterized by X-ray diffraction and scanning electron microscope; the electrochemical performance of the sensor was studied by cyclic voltammetry and chronoamperometry. The sensor had a sensitivity of 1949.1 μµA·L/（mmol·cm2）for glucose detection in the linear range of 1.0-8000 μµmol/L at a potential of 0.55 V,and the detection limit was 0.2 μµmol/L. The sensor was also applied to measure the concentration of glucose in serum samples. The developed nanocomposites sensor has the potential prospect to monitor blood glucose. © 2023, Youke Publishing Co.,Ltd. All rights reserved.     

Flow-injection chemiluminescence determination of tryptophan using galangin-potassium permanganate–polyphosphoric acid system

A high sensitive flow-injection chemiluminescence （FI-CL） method for the determination of tryptophan has been developed. The method is based on the chemiluminescence reaction of galangin-potassium permanganate-tryptophan in polyphosphoric acid （PPA） media. Under the optimized conditions, tryptophan was determined in the range 0.05-10 μg/mL with the detection limit （3tr） of 5.0 × 10^-3 μg/mL. The relative standard deviation （RSD） was 1.0% for 11 replicate determinations of 1.0 μg/mL tryptophan. Three synthetic samples were determined selectively with recoveries in the range from 99.6% to 102.0% in the presence of other amino acids.