Magnetic solid phase extraction and determination of polychlorinated biphenyls in beverages utilizing C60 modified magnetic polyamido-amine dendrimers in combination with gas chromatography-tandem mass spectrometry.

Polychlorinated biphenyls (PCBs) are persistent organic pollutants which are widely present in environment and harmful to human health. In this study, an efficient and convenient magnetic solid phase extraction method with C60 modified magnetic polyamido-amine (PAMAM) dendrimers as sorbents was established for enriching trace amounts of PCBs in beverage samples. Gas chromatography-tandem mass spectrometry (GC-MS/MS) was utilized for analysis of PCBs. Parameters affecting extraction efficiency were optimized. Under optimal parameters, good linearity can be achieved in concentration range of 0.001-20 µg L-1 and 0.002-20 µg L-1 for nine selected PCBs. The limits of detection for PCBs were in the range of 0.1-0.2 ng L-1. The spiked recoveries were in the range of 87.0 %-115.1 % (n = 3). The results proved that this established method was reliable for monitoring trace PCBs in beverage samples.

Novel electrochemical sensor from magnetic carbon dots and cetyltrimethylammonium bromide for sensitive measurement of tetrabromobisphenol A in beverages.

Present work depicted a novel electrochemical sensor fabricated with magnetic carbon dots (M-CDs) and cetyltrimethylammonium bromide (CTAB) modified glassy carbon electrode (GCE) for selective measurement of 3,3',5,5'-tetrabromobisphenol A (TBBPA) in beverages. The M-CDs composite material revealed good electrocatalytic activity, and CTAB has strong hydrophobic interaction which enable it have good enrichment capacity of hydrophobic compounds, and combination of them further enhances the electrochemical signal. Hence CTAB decoration can markedly improve the detection performance of TBBPA. Electrochemical properties of the fabricated sensor was investigated through performing cyclic voltammetry (CV). The morphology and functional groups of the modified materials were examined with transmission electron microscope (TEM) and Fourier transform infrared spectroscopy (FTIR). The results indicated that the synthesized material had a spherical-like structure, good dispersion properties and plenty of functional groups on the surface. The effects of incubation potential, incubation time, pH of electrolyte, and scanning rate on oxidation peak current were investigated. Under optimal conditions, the designed sensor had good linear range of 1 nM-1000 nM, and the detection of limit of the constructed sensor was 0.75 nM. The constructed sensor was utilized to detect TBBPA in vitamin water, scream drink and genki forest, and satisfactory detection performance had been achieved.

Sensitive determination of polychlorinated biphenyls from beverages based on switchable solvent microextraction: A robust methodology.

Polychlorinated biphenyls (PCBs) are a kind of hazardous persistent organic contaminants and widely present in nature due to large consumption in the past. Although PCBs have been banned in many countries of the world, they are still present at trace level in food and water samples. It is of significant value to establish reliable enrichment and detection method. Based on the conversion of the hydrophilicity and hydrophobicity from heptanoic acid under alkali and acid, increasing the contact area between heptanoic acid and PCBs, a new switchable solvent micro-extraction method for PCBs from beverages was developed with good extraction efficiency using heptanoic acid as the extractant prior to gas chromatography-tandem mass spectrometry (GC-MS/MS). The key parameters that had impact on enrichment of PCBs were investigated in detail. Under the optimal conditions, a good linearity can be achieved in a concentration range of 0.01-20 µg L-1 with the correlation coefficients of 0.9978-0.9994. Limits of detection for PCB28, PCB53, PCB206 were 3 ng L-1 and PCB118 was 5 ng L-1 while other target PCBs were 2 ng L-1. Intra-day and inter-day precisions were in the range of 1.9-4.2% and 2.1-4.2％(relative standard deviation, RSD, n = 6), respectively. The real sample spiked recoveries of the targets were in the range of 93.2-114.3％ (n = 3). The enrichment factors were in the range of 16.2-17.9. The results proved that this method was reliable for monitoring trace PCBs in beverage samples and will help for future assessments of impacts on human and animal health.

Graphene oxide modified magnetic polyamidoamide dendrimers based magnetic solid phase extraction for sensitive measurement of polycyclic aromatic hydrocarbons.

In this study, graphene oxide modified magnetic polyamidoamine dendrimers (MNPs@PAMAM-G2.0@GO) nanoparticles were successfully prepared by amidation method. The obtained MNPs@PAMAM-G2.0@GO nanocomposites were examined by fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), vibrating sample magnetometer (VSM), scanning electron microscope (SEM) and transmission electron microscopy (TEM), etc. MNPs@PAMAM-G2.0@GO exhibited excellent adsorption property and was investigated for magnetic solid phase extraction (MSPE) of polycyclic aromatic hydrocarbons (PAHs) from water. The detection of extracted PAHs was accomplished by high performance liquid chromatography (HPLC) and gas chromatography tandem mass spectrometry (GC-MS/MS). The target PAHs included anthracene (ANT), pyrene (PYR), fluoranthene (FLT), carbazole (CB), 7-methylquinoline (7-MQL), 9-methylcarbazole (9-MCB), dibenzothiophene (DBT) and 4,6-dimethyldibenzothiophene (4,6-DBT). Important operation parameters for MSPE that could affect the extraction efficiencies of PAHs were investigated in detail. Under optimal parameters, the constructed method demonstrated excellent linear range with 0.001-10 µg L-1 for analytes and low limits of detection within the range of 0.11-0.9 ng L-1. The spiked average recoveries of PAHs in natural water samples ranged from 92.5% to 105.2%. The promising results indicated that MNPs@PAMAM-G2.0@GO could be employed to efficiently extract PAHs from aqueous samples.

Preparation of Polyamidoamine Dendrimer Modified Magnetic Nanoparticles and Its Application for Reliable Measurement of Sudan Red Contaminants in Natural Waters at Parts-Per-Billion Levels.

The health threat from Sudan red dyes has been the subject of much attention in recent years and is crucial to design and establish reliable measurement technologies. In the present study, a new magnetic nanomaterial, polyamidoamine dendrimer-modified magnetic nanoparticles (Gn-MNPs), was synthesized and characterized. The nanomaterials had good adsorption capacity for Sudan dyes from natural waters. G1.5-MNPs possessed excellent adsorption capacity and a linear adsorption relationship over the range from 0.02 to 300 µg L-1 of Sudan dyes with relative coefficients all larger than 0.996. The sensitivity of the proposed method was excellent with detection limits over the range from 1.8 to 5.5 ng L-1 and the precision was less than 3.0%. G1.5-MNPs showed a remarkable application potential for the enrichment of trace environment pollutants in aqueous samples and the developed method based on this nanomaterial could be a robust and reliable alternative tool for routine monitoring of such pollutants.

Selective detection of Cu2+ using nitrogen-doped carbon dots derived from humic acid and urea based on specific inner filter effect.

A new kind of nitrogen-doped carbon dots (N-CDs) was synthesized via a simple hydrothermal strategy using humic acid as the carbon source and urea as the nitrogen source. The fluorescence intensity of as-prepared N-CDs was quenched significantly in presence of Cu2+ based on a specific inner filter effect, which could be utilized to construct a selective sensor for monitoring Cu2+ in aqueous samples. The sensor exhibited good linearity over the range of 0.1-2 µM, and high sensitivity with a detection limit of 25 nM. Under the optimal conditions, there was no significant interference by other metal ions such as Cd2+, Al3+, Cr3+, Fe3+, Pb2+, Na+, Ni+, Fe2+, Ba2+, Ca2+, Co2+, Mg2+, As3+, K+, Zn2+ for Cu2+ detecting except Hg2+.The interference of Hg2+ can be masked by addition of sodium chloride. The experimental results demonstrated that the prepared N-CDs owned strong fluorescence, high monodispersity, good stability and good water solubility, and the constructed sensor had many advances and great application prospect in environmental field.

Sensitive detection of 2,4,6-trinitrotoluene utilizing fluorescent sensor from carbon dots and reusable magnetic core-shell nanomaterial.

Carbon dots have been a promising nano-carbon material with many advantages, and attracted many more attentions. This study designed a new chemosensor integrating the strong fluorescent property of carbon dots and the magnetism of amino-functionalized magnetic core-shell nanomaterial, Fe@SiO2-NH2 for determination of 2,4,6-trinitrotoluene (TNT). In this system, fluorescent carbon dots interacted with amino groups on the surface of amino-functionalized magnetic core-shell nanomaterial leading to fluorescence quenching of carbon dots, appearance of TNT competitively replaced of carbon dots on the surface of the magnetic material through forming a Meisenheimer complex. This sensor exhibits excellent selectivity and sensitivity for TNT, and which provided a good dynamic linear range for TNT from 10 to 2000 ng mL-1. The experiments demonstrate a low detection limit of 2.15 ng mL-1. The intra-day precisions for 25, 100 and 500 ng mL-1 were 4.6, 2.3 and 0.5% (RSD, n = 6), inter-day precisions for 25, 100 and 500 ng mL-1 were 4.2, 2.5 and 0.9% (RSD, n = 6), respectively. The developed sensor was validated with river water, dust, and soil samples, and the achieved spiked recoveries were immensely satisfied from 98.1% to 102.0%. The Fe@SiO2-NH2 possessed excellent reusability. This sensor exhibits that it is simple, sensitive and selective, and will be a vital analytical tool for TNT in many fields.

Highly selective fluorescence sensor sensing benzo[a]pyrene in water utilizing carbon dots derived from 4-carboxyphenylboronic acid.

4-Carboxyphenylboronic acid was used as the single precursor to facilely prepare fluorescent carbon quantum dots by one-step solvothermal method. The as-obtained carbon dots (CDs) exhibited highly selective and sensitive for benzo[a]pyrene (BaP), and may be a splendid sensor for sensing BaP. The principle was that the as-prepared CDs could form a complex with BaP through hydrophobic interaction which causes the decrease of fluorescence intensity of CDs by static quenching principle. The constructed fluorescent sensor exhibited excellent linearity ranged from 0.002 to 0.06 µg mL-1 and provided a low limit of detection of 0.16 ng mL-1. The experimental results showed that this fluorescent sensor resulted in simplicity, rapidness, low cost, short analytical time, and high sensitivity and stability. Validation with real water samples endowed the sensor high reliability and feasibility for BaP determination in practical application in various samples.

Rapid magnetic enrichment and sensitive detection of Sudan pollutants with nanoscale zero valent iron-based nanomaterials in combination with liquid chromatography-ultraviolet detector.

In present work, we reported a new nanomaterial nano Fe0 decorated with SiO2 and dopamine by self-assembly method (Fe@SiO2@PDA). A sensitive method for determination of Sudan pollutants in aqueous samples was developed using Fe@SiO2@PDA as magnetic solid phase extraction adsorbents prior to high-performance liquid chromatography with variable wavelength detector. The possible parameters which would affect the enrichment have been optimized. The best parameters were as follows: elutent, 4.5 mL methanol; adsorbent dosage, 30 mg; adsorption time, 20 min; elution time, 18 min; sample pH 7; sample volume, 40 mL. The experimental results demonstrated that Fe@SiO2@PDA exhibited good adsorption properties to Sudan Red dyes. The established method provided excellent linear ranges over 0.01-50 µg L-1 and detection limits ranged from 2.0 to 5.1 ng L-1 for Sudan red I-IV. The developed method was also evaluated with real water samples and the results demonstrated that it was of applicative value owing to its merits including robustness, easy operation, fastness, cheapness and high enrichment efficiency, and had great prospect in environmental fields.

Magnetic polyamidoamine dendrimers for magnetic separation and sensitive determination of organochlorine pesticides from water samples by high-performance liquid chromatography.

Organochlorine pesticides (OCPs) have received much attention due to their toxicity. Reliable methods to monitor their residues in the environment are needed. Here, magnetic polyamidoamine dendrimers were prepared by co-precipitation, Michael addition, and amidation. The magnetic polyamidoamine dendrimers demonstrated good adsorption ability for OCPs-this feature was utilized to construct a sensitive tool for monitoring OCPs in water samples. The proposed method provided remarkable linearity from 0.1 to 500 µg/L and satisfactory limits of detection from 0.012 to 0.029 µg/L. The spiked recoveries of the four target analytes were 91.8%-103.5% with relative standard deviations less than 4.5%. The magnetic materials had good reusability. The results indicated that the resulting method was an efficient, easy, rapid, economical, and eco-friendly tool for monitoring OCPs in aqueous samples.

Magnetic polyamidoamine dendrimer grafted with 4-mercaptobenzoic acid as an adsorbent for preconcentration and sensitive determination of polycyclic aromatic hydrocarbons from environmental water samples.

Polyamidoamine dendrimer decorated Fe3O4 magnetic nanoparticles was synthesized and grafted with 4-mercaptobenzoic acid (4-MBA). The resulting material was utilized to develop an effective magnetic solid phase extraction method in combination with high performance liquid chromatography for trace determination of polycyclic aromatic hydrocarbons including phenanthrene (PHE), anthracene (ANT), fluoranthene (FLT), pyrene (PYR) and benzo(a)pyrene (BaP). The MNPs@G3.0@4-MBA exhibited to be an efficient extracting medium due to the existence of terminal benzene ring groups, the internal pores, and strong hydrophobic interactions and π-π interactions. The experiments demonstrated that the proposed method possessed excellent linearity in the concentration range of 0.1-300 µg L-1 with correlation coefficients (R) larger than 0.997, and the limits of detection (LODs, S/N = 3) according to the ratio of signal to noise equal to three of PHE, ANT, FLT, PYR and BaP were 0.014 µg L-1, 0.032 µg L-1, 0.055 µg L-1, 0.027 µg L-1 and 0.039 µg L-1, respectively. The proposed method was applied to real water samples and the spiked recoveries were over the range of 92-99%. The results showed that the method earned good repeatability and high sensitivity, and the as-prepared materials were stable and reusable, which displayed that the proposed method would have a wonderful application prospect.

A reliable and facile fluorescent sensor from carbon dots for sensing 2,4,6-trinitrophenol based on inner filter effect.

2,4,6-Trinitrophenol (TNP) has absorbed much concerns because of its toxic effect and threat on the environment, which results from the fact that it is an important and universal reagent widely utilized for manufacturing many products. It is of great necessity to explore facile and efficient methods for monitoring TNP. In present study, carbon dots (CDs), a new carbonaceous nanomaterial with strong fluorescence, was applied to build a novel sensor for highly sensitive and selective detection of TNP. In the sensing procedure, the fluorescence intensity of as-prepared CDs was diminished with the presence of TNP due to inner filter effect (IFE) quenching mechanism. The sensitivity of the fluorescent sensor was very high with limit of detection down to 5.37 ng mL-1. This fluorescent sensor was evaluated and excellent spiked recoveries were gained, which demonstrated that the developed sensor would be a robust tool for environmental applications.

g-C3N4- and polyaniline-co-modified TiO2 nanotube arrays for significantly enhanced photocatalytic degradation of tetrabromobisphenol A under visible light.

An ordered g-C3N4- and polyaniline-modified titanium oxide nanotube array (g-C3N4- and PANI-co-modified TiO2 NTAs) was successfully synthesized and used as a photocatalyst. Polyaniline (PANI) was coated onto TiO2 NTAs by electrochemical polycondensation, and g-C3N4 was deposited via the soaking adsorption method. The photocatalysts were examined by several technologies. The experiments demonstrated that the amount of g-C3N4 and PANI, as well as the initial pH value, had significant effects on the photocatalytic efficiency. The resulting photocatalysts exhibited high visible light photocatalytic ability for tetrabromobisphenol A (TBBPA) for two reasons. First, PANI expanded the light absorption into the visible region. Second, rapid and efficient separation of photoinduced charges from the photogenerated potential difference were produced at the contact interface of g-C3N4 and PANI-co-modified TiO2 NTAs. The •OH, [Formula: see text] and h+ were dominant components for the photocatalytic degradation of TBBPA. In addition, the g-C3N4 and PANI-co-modified TiO2 NTAs have excellent long-term stability.