scholarly journals Magnetic Mesoporous Silica Composite for Enhanced Preconcentration of Selected Organophosphorus Pesticides in Fruits

2020 ◽  
Vol 20 (4) ◽  
pp. 729 ◽  
Author(s):  
Nur Husna Zainal Abidin ◽  
Wan Nazihah Wan Ibrahim ◽  
Nor Suhaila Mohamad Hanapi ◽  
Nor’ashikin Saim
Keyword(s):  
Electron Microscopy ◽  
High Performance ◽  
Magnetic Particles ◽  
Solid Phase ◽  
Organophosphorus Pesticides ◽  
Magnetic Solid Phase Extraction ◽  
High Concentration ◽  
Relative Standard ◽  
Fruit Samples ◽  
Mcm 41

In the present work, MCM-41 coated magnetic particles (Fe3O4-MCM-41) composite was synthesized and employed as an effective adsorbent in magnetic solid phase extraction (MSPE) of three selected organophosphorus pesticides (OPPs) namely chlorpyrifos, diazinon and parathion methyl from grape and strawberry samples prior to high performance liquid chromatography with UV detection (HPLC-UV). The synthesized sorbent was physicochemically and morphologically characterized via Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and N2 adsorption analysis. The main parameters on the extraction efficiency of selected OPPs, including extraction time, desorption solvent, desorption time, and sorbent dosage, were thoroughly optimized. Compared to MCM-41 sorbent, the newly synthesized Fe3O4-MCM-41 adsorbent shows a linear response (0.1-5.00 mg L–1) with good determination coefficients ranging from 0.9900 to 0.9980, low limits detection (LODs), 0.02-0.15 mg L–1 and low limit quantifications (LOQs), 0.06-0.40 mg L–1. The precision as relative standard deviation (%RSD) of the proposed MSPE method was studied at low and high concentration (0.1-5.0 mg L–1) based on intra-day (1.0 to 6.0%, n = 3) and inter-day (1.0 to 7.0%, n = 3), respectively. Fruit matrices were used to assess the field applicability of the sorbents. Comparatively, Fe3O4-MCM-41 achieved excellent percent recovery (85–120%) compared to the MCM-41 (70–110%). The result revealed that the Fe3O4-MCM-41 composite was efficient sorbent with good capability for the preconcentration of selected OPPs from fruit samples.

scholarly journals Magnetic Solid Phase Extraction using Magnetic Mesoporous Silica for Preconcentration of Organophosphorus Pesticides

2019 ◽  
Vol 8 (4) ◽  
pp. 6847-6852
Keyword(s):  
Mesoporous Silica ◽  
Solid Phase Extraction ◽  
Water Samples ◽  
High Performance ◽  
Solid Phase ◽  
Organophosphorus Pesticides ◽  
Magnetic Solid Phase Extraction ◽  
Phase Extraction ◽  
Magnetic Solid ◽  
Mcm 41

The present study describes the synthesis, characterization and application of two mesoporous silica material based coated magnetic nanoparticles namely Fe3O4 -SBA-15 and Fe3O4 -MCM-41 for the simultaneous preconcentration of three selected organophosphorus pesticides (OPPs) namely chlorpyrifos, diazinon and parathion methyl from water samples. The resultant sorbent material was physicochemically and morphologically characterized by field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD) and N2 adsorption analysis. OPPs pesticides extraction efficiency of two sorbents were evaluated through magnetic solid phase extraction (MSPE) using high performance liquid chromatography with ultraviolet detector (HPLC/UV). The main parameters affecting the sorbent efficiency namely extraction time and desorption solvent were optimized. Comparatively, Fe3O4 -SBA-15 achieved excellent percent recovery (97.5%) compared to the Fe3O4 -MCM-41 (87.1%) under optimum condition respectively. The result appealed that the Fe3O4 -SBA-15 composite was efficient sorbent with good capability for the preconcentration of selected OPPs from water samples.AThe present study describes the synthesis, characterization and application of two mesoporous silica material based coated magnetic nanoparticles namely Fe3O4 -SBA-15 and Fe3O4 -MCM-41 for the simultaneous preconcentration of three selected organophosphorus pesticides (OPPs) namely chlorpyrifos, diazinon and parathion methyl from water samples. The resultant sorbent material was physicochemically and morphologically characterized by field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD) and N2 adsorption analysis. OPPs pesticides extraction efficiency of two sorbents were evaluated through magnetic solid phase extraction (MSPE) using high performance liquid chromatography with ultraviolet detector (HPLC/UV). The main parameters affecting the sorbent efficiency namely extraction time and desorption solvent were optimized. Comparatively, Fe3O4 -SBA-15 achieved excellent percent recovery (97.5%) compared to the Fe3O4 -MCM-41 (87.1%) under optimum condition respectively. The result appealed that the Fe3O4 -SBA-15 composite was efficient sorbent with good capability for the preconcentration of selected OPPs from water samples.

scholarly journals Magnetic Micro-Solid-Phase Extraction Using a Novel Carbon-Based Composite Coupled with HPLC–MS/MS for Steroid Multiclass Determination in Human Plasma

Molecules ◽  
2021 ◽  
Vol 26 (7) ◽  
pp. 2061
Author(s):  
Andrea Speltini ◽  
Francesca Merlo ◽  
Federica Maraschi ◽  
Giorgio Marrubini ◽  
Anna Faravelli ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Solid Phase Extraction ◽  
Human Plasma ◽  
High Performance ◽  
Solid Phase ◽  
Magnetic Solid Phase Extraction ◽  
Bet Surface Area ◽  
Phase Extraction ◽  
Sensitivity Matrix ◽  
Relative Standard

A micron-sized sorbent, Magn-Humic, has been prepared by humic acids pyrolysis onto silica-coated magnetite. The material was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS), thermogravimetric analysis (TGA), and Brunauer, Emmett, and Teller (BET) surface area measurements and applied for simultaneous magnetic solid-phase extraction (MSPE) of glucocorticoids, estrogens, progestogens, and androgens at ng mL−1 levels from human plasma followed by high-performance liquid chromatography coupled with mass spectrometry (HPLC–MS/MS). Due to the low affinity for proteins, steroids extraction was done with no need for proteins precipitation/centrifugation. As highlighted by a design of experiments, MSPE was performed on 250 µL plasma (after 1:4 dilution) by 50 mg Magn-Humic (reusable for eight extractions) achieving quantitative recovery and satisfying clean-up. This was improved by washing (2 mL 2% v/v formic acid) prior to analytes elution by 0.5 mL 1:1 v/v methanol-acetonitrile followed by 0.5 mL methanol; eluate reduction to 0.25 mL compensated the initial sample dilution. The accuracy was assessed in certified blank fetal bovine serum and in human plasma, gaining satisfactory recovery in the range 65–122%, detection limits in the range 0.02–0.3 ng mL−1 (0.8 ng mL−1 for 17-β-estradiol) and suitable inter-day precision (relative standard deviation (RSD) <14%, n = 3). The method was evaluated in terms of selectivity, sensitivity, matrix-effect, instrumental carry-over, and it was applied to human plasma samples.

scholarly journals In Situ Synthesis of a Magnetic Graphene Platform for the Extraction of Benzimidazoles from Food Samples and Analysis by High-Performance Liquid Chromatography

2017 ◽  
Vol 2017 ◽  
pp. 1-11 ◽  
Author(s):  
Qianchun Zhang ◽  
Yulan Liu ◽  
Xingyi Wang ◽  
Huimin Li ◽  
Junyu Chen
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Solid Phase ◽  
Correlation Coefficients ◽  
Magnetic Solid Phase Extraction ◽  
Food Samples ◽  
Magnetic Graphene ◽  
Relative Standard

A novel method was proposed for the determination of five benzimidazoles (oxfendazole, mebendazole, flubendazole, albendazole, and fenbendazole) using magnetic graphene (G-Fe3O4). G-Fe3O4 was synthesized via in situ chemical coprecipitation. The properties of G-Fe3O4 were characterized by various instrumental methods. G-Fe3O4 exhibited a great adsorption ability and good stability towards analytes. Various experimental parameters that might affect the extraction efficiency such as the amount of G-Fe3O4, extraction solvent, extraction time, and desorption conditions were evaluated. Under the optimized conditions, a method based on G-Fe3O4 magnetic solid-phase extraction coupled with high-performance liquid chromatography was developed. A good linear response was observed in the concentration range of 0.100–100 μg/L for the five benzimidazoles, with correlation coefficients ranging from 0.9966 to 0.9998. The limits of detection (S/N=3) of the method were between 17.2 and 32.3 ng/L. Trace benzimidazoles in chicken, chicken blood, and chicken liver samples were determined and the concentrations of oxfendazole, mebendazole, flubendazole, and fenbendazole in these samples were 13.0–20.2, 1.62–4.64, 1.94–6.42, and 0.292–1.04 ng/g, respectively. The recovery ranged from 83.0% to 115%, and the relative standard deviations were less than 7.9%. The proposed method was sensitive, reliable, and convenient for the analysis of trace benzimidazoles in food samples.

scholarly journals Amine-functionalized magnetic activated carbon as an adsorbent for preconcentration and determination of acidic drugs in environmental water samples using HPLC-DAD

2020 ◽  
Vol 18 (1) ◽  
pp. 1218-1229 ◽  
Author(s):  
Mpingana Ndilimeke Akawa ◽  
Kgogobi Mogolodi Dimpe ◽  
Philiswa Nosizo Nomngongo
Keyword(s):  
Activated Carbon ◽  
River Water ◽  
Water Samples ◽  
High Performance ◽  
Solid Phase ◽  
Magnetic Solid Phase Extraction ◽  
Array Detector ◽  
Acidic Drugs ◽  
Relative Standard

AbstractIn the present study, a convenient and highly effective method was developed for the quantification of acidic drugs in wastewater and river water samples. Ultrasonic-assisted magnetic solid phase extraction employing magnetic waste tyre-based activated carbon nanocomposite functionalized with [3-(2-aminoethylamino)propyl]trimethoxysilane as a cost-effective and efficient adsorbent was used for the extraction and preconcentration of acidic drugs (naproxen [NAP], ketoprofen (KET) and diclofenac [DIC]). The quantification of target analytes was achieved by high‐performance liquid chromatography with diode array detector. Under optimum conditions, the detection limit, quantification limit and relative standard deviation obtained for the analytes of interest ranged from 0.38 to 0.76, 1.26 to 2.54 µg L−1 and 2.02 to 4.06%, respectively. The applicability of the developed method was assessed by the spike recovery tests and the relative recoveries proved that the method is reliable for the determination of acidic drugs in wastewater. Thereafter, the method was applied successfully for the determination of NAP, KET and DIC in river water, influent and effluent wastewater.

scholarly journals Pre-Concentration and Determination of Tetracyclines Antibiotics Residues in Water Samples Using RGO/Fe3O4 Nanocomposite as Extraction Sorbent

2021 ◽  
Vol 21 (5) ◽  
pp. 1196
Author(s):  
Ungku Amirul Arif Ungku Abdullah ◽  
Nor Suhaila Mohamad Hanapi ◽  
Wan Nazihah Wan Ibrahim ◽  
Nursyamsyila Mat Hadzir ◽  
Nurzaimah Zaini ◽  
...  
Keyword(s):  
Water Samples ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Magnetic Solid Phase Extraction ◽  
Coefficient Of Determination ◽  
Array Detector ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Magnetic Solid

Existing methods used in tracing Tetracyclines' antibiotics (TCAs) residues which pose serious environmental problems, consume high amounts of organic solvents, are time-consuming, and are relatively expensive. A simple and effective magnetic solid-phase extraction (MSPE) based on reduced graphene oxide/magnetite (RGO/Fe3O4) nanocomposite sorbent was successfully developed for preconcentration and extraction of TCAs residues from water samples. The analytes were determined by high-performance liquid chromatography with a diode-array detector (HPLC-DAD). The synthesized nanocomposite was characterized using Fourier-transform infrared spectroscopy (FTIR), X-ray diffractometry (XRD), and field emission scanning electron microscopy (FESEM). Sample pH, amount of adsorbent, sample volume, extraction time, desorption time, and desorption solvent were evaluated and optimized. Under optimized conditions, the method demonstrated good linearity over the concentration range of 0.05–1.0 mg L–1 with the coefficient of determination (R2) ≥ 0.9978. Limit of detection (LOD) and limit of quantification (LOQ) were 0.006–0.011 mg L–1 and 0.019–0.036 mg L–1, respectively. The accuracy and precision of the developed method were proven by good analyte recovery (89.77–106.33%) and acceptable precision with relative standard deviation, RSD ≤ 5.54%. The results showed that magnetic solid RGO/Fe3O4 could be a suitable adsorbent in the preconcentration and extraction of TCAs in water samples.

scholarly journals Control of Organophosphorus Pesticides Residues in Honey Samples Using a Miniaturized Tandem Preconcentration Technique Coupled with High Performance Liquid Chromatography

2020 ◽  
Vol 26 (1) ◽  
pp. 52-60
Author(s):  
Ali Mohebbi ◽  
Saeid Yaripour ◽  
Mir Ali Farajzadeh ◽  
Mohammad Reza Afshar Mogaddam ◽  
Hassan Malekinejad
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Solid Phase ◽  
Organophosphorus Pesticides ◽  
Sample Pretreatment ◽  
Experimental Conditions ◽  
Suggested Approach ◽  
Pesticides Residues ◽  
Relative Standard

Background : In the present work, a miniaturized sample preparation method based on combination of dispersive solid phase extraction and temperature–induced homogenous liquid–liquid microextraction has been proposed for the extraction and preconcentration of some organophosphorus pesticides (parathion–methyl, triazophos, parathion, diazinon, and phoxim) from honey samples prior to their analysis by high performance liquid chromatography–ultraviolet detection. Methods: In this method, initially the analytes were adsorbed onto a sorbent (C18) and then desorbed by the use of cyclohexyl amine as an eluent. In the next step, the eluent was mixed with water thermostated at 0 °C to obtain a homogenous solution. By increasing the temperature, the solubility of cyclohexyl amine in water was decreased and led to formation of dispersed fine droplets in the whole of solution. These droplets go up through the solution and collected on top of the solution. Finally, an aliquot of the organic phase was sucked in a microsyringe and injected into the separation system for analysis. Results: Under the optimum experimental conditions, limits of detection and quantification were calculated to be in the ranges of 0.90–1.75 and 3.0–5.8 ng g–1 in honey samples, respectively. Enrichment factors and extraction recoveries were in the ranges of 148–183 and 59–73%, respectively. The relative standard deviations varied from 2–4% and 4–5% for intra– (n = 6) and inter–day (n = 4) precisions, respectively. Conclusion: The suggested approach was satisfactorily utilized to the analysis of 21 honey samples. The proposed miniaturized tandem sample pretreatment method enhanced the sensitivity of the instrumental analysis.

Determination of four parabens in cosmetics by high-performance liquid chromatography with magnetic solid-phase and ionic dispersive liquid–liquid extraction

2021 ◽  
Vol 40 (1) ◽  
pp. 161-172
Author(s):  
Xun Gao ◽  
Kai Xu ◽  
Miaomiao Chi ◽  
Jiaojiao Li ◽  
Lingzhe Suo ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Trace Amount ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Magnetic Solid Phase Extraction ◽  
Nano Materials ◽  
Extraction Solvent ◽  
Magnetic Solid ◽  
Dispersive Liquid Liquid Microextraction

Abstract To determine the trace amount of four benzoic acid esters in cosmetics, ionic dispersive liquid–liquid microextraction (DLLME) and magnetic solid-phase extraction were combined and optimized. After solvent optimization, 1-octyl-3-methylimidazolium hexafluorophosphate was selected as the extraction solvent to form hydrophobic droplets in the process of ionic DLLME, followed by removal of ions from the sample solution containing Fe3O4@GO nano-materials. The magnetic nano-materials were characterized using Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy, and vibrating sample magnetometer. Some parameters affecting the efficiency of extraction were optimized using Box-Behnken design. Under optimized conditions, the limit of detection for all the preservatives was less than 0.135 mg/L and the accuracy ranged from 88.5% to 101%. This technology could determine the trace amount of preservatives in cosmetics with comparatively higher accuracy and sensitivity.

Calcium/Copper alginate framework doped with CuO nano-particles as a novel adsorbent for micro-extraction of benzodiazepines from human serum

2020 ◽  
Vol 16 ◽  
Author(s):  
Nadereh Rahbar ◽  
Fatemeh Ahmadi ◽  
Zahra Ramezani ◽  
Masoumeh Nourani
Keyword(s):  
Human Serum ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Nano Particles ◽  
Limit Of Quantification ◽  
Analytical Methodology ◽  
Fiber Fabrication ◽  
Relative Standard ◽  
Green Procedure

Background: Sample preparation is one of the most challenging phases in pharmaceutical analysis, especially in biological matrices, affecting the whole analytical methodology. Objective: In this study, a new Ca(II)/Cu(II)/alginate/CuO nanoparticles hydrogel fiber (CCACHF) was synthesized through a simple, green procedure and applied for fiber micro solid phase extraction (FMSPE) of diazepam (DIZ) and oxazepam (OXZ) as model drugs prior to high-performance liquid chromatography-UV detection (HPLC-UV). Methods: Composition and morphology of the prepared fiber were characterized and the effect of main parameters on the fiber fabrication and extraction efficiency have been studied and optimized. Results: In optimal conditions, calibration curves were linear ranging between 0.1–500 µg L−1 with regression coefficients of 0.9938 and 0.9968. Limit of detection (LOD) (S/N=3) and limit of quantification (LOQ) (S/N=10) of the technique for DIZ and OXZ were 0.03 to 0.1 µg L−1. Within-day and between-day relative standard deviations (RSDs) for DIZ and OXZ were 6.0–12.5% and 3.3–9.4%, respectively. Conclusion: The fabricated adsorbent has been substantially employed to extraction of selected benzo-diazepines (BZDs) from human serum real specimens and the obtained recoveries were also satisfactory (82.1-109.7%).

Sign in / Sign up

Export Citation Format

Share Document