scholarly journals Polythiophene-Chitosan Magnetic Nanocomposite as a Highly Efficient Medium for Isolation of Fluoxetine from Aqueous and Biological Samples

2016 ◽  
Vol 2016 ◽  
pp. 1-11 ◽  
Author(s):  
Alireza Feizbakhsh ◽  
Amir Hossein Mohsen Sarrafi ◽  
Shokooh Ehteshami
Keyword(s):  
Biological Samples ◽  
Solid Phase ◽  
Correlation Coefficients ◽  
Current Method ◽  
Magnetic Solid Phase Extraction ◽  
Sample Volume ◽  
Magnetic Nanocomposite ◽  
Extraction Time ◽  
Human Blood Plasma ◽  
Solution Ph

Polythiophene/chitosan magnetic nanocomposite as an adsorbent of magnetic solid phase extraction was proposed for the isolation of fluoxetine in aqueous and biological samples prior to fluorescence detection at 246 nm. The synthesized nanoparticles, chitosan and polythiophene magnetic nanocomposite, were characterized by scanning electron microscopy, FT-IR, TGA, and EDAX. The separation of the target analyte from the aqueous solution containing the fluoxetine and polythiophene/chitosan magnetic nanocomposite was simply achieved by applying external magnetic field. The main factors affecting the extraction efficiency including desorption conditions, extraction time, ionic strength, and sample solution pH were optimized. The optimum extraction conditions were obtained as 10 min for extraction time, 25 mg for sorbent amount, 50 mL for initial sample volume, methanol as desorption solvent, 1.5 mL for desorption solvent volume, 3 min for desorption time, and being without salt addition. Under the optimum conditions, good linearity was obtained within the range of 15–1000 μg L−1for fluoxetine, with correlation coefficients 0.9994. Furthermore, the method was successfully applied to the determination of fluoxetine in urine and human blood plasma samples. Compared with other methods, the current method is characterized with highly easy, fast separation and low detection limits.

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 Quantitative Determination of Fluoroquinolones in Contaminated Soils by HPLC with Solid-Phase Extraction

2020 ◽  
Vol 17 (1) ◽  
pp. 0048
Author(s):  
Bashar hussin Qassim
Keyword(s):  
Solid Phase Extraction ◽  
Contaminated Soils ◽  
Solid Phase ◽  
Correlation Coefficients ◽  
Current Method ◽  
Phase Extraction ◽  
Soil Matrix ◽  
Extraction Solvent ◽  
Relative Standard ◽  
Hplc Detector

This work reports the development of an analytical method for the simultaneous analysis of three fluoroquinolones; ciprofloxacin (CIP), norfloxacin (NOR) and ofloxacin (OFL) in soil matrix. The proposed method was performed by using microwave-assisted extraction (MAE), solid-phase extraction (SPE) for samples purification, and finally the pre-concentrated samples were analyzed by HPLC detector. In this study, various organic solvents were tested to extract the test compounds, and the extraction performance was evaluated by testing various parameters including extraction solvent, solvent volume, extraction time, temperature and number of the extraction cycles. The current method showed a good linearity over the concentration ranging from 1 – 300ng g-1 with correlation coefficients (r2 > 0.998) for all test compounds. Good recoveries were also obtained for the test compounds ranged from 89 – 99 %. The relative standard deviation (RSD) from intra-day and inter-day precision was lower than 7%, and the detection (LOD) and quantification (LOQ) limits ranged from 0.9 – 2.7ng g-1.Finally, the proposed method was applied to determine the target compounds in real soil samples irrigated with wastewater. The results confirm the presence of the test compounds in soils with values ranging from 1.9 – 4.6ng g-1, as well as the suitability of the proposed method to determine the test compounds in real soil matrix as well as the ability of the test compounds to accumulate in soils irrigated with sewage.

scholarly journals Atrazine and 2, 4-D determination in corn samples using microwave assisted extraction and on-line solid-phase extraction coupled to liquid chromatography.

2018 ◽  
Vol 62 (2) ◽  
Author(s):  
Ana Susana Santos-Hernández ◽  
Laura Hinojosa-Reyes ◽  
Isabel del Carmen Sáenz-Tavera ◽  
Aracely Hernández-Ramírez ◽  
Jorge Luis Guzmán-Mar
Keyword(s):  
Solid Phase Extraction ◽  
Solid Phase ◽  
Monolithic Column ◽  
Correlation Coefficients ◽  
Sample Pretreatment ◽  
Enrichment Factors ◽  
Sample Volume ◽  
Phase Extraction ◽  
Microwave Assisted ◽  
On Line

<p>On-line sample pretreatment (clean-up and analyte preconcentration) was coupled to sequential injection chromatography for the determination of 2, 4-D (2,4-dichlorophenoxyacetic acid) and atrazine in corn samples. Prior to their analysis, microwave-assisted approach was evaluated and optimized for the extraction of 2,4-D and atrazine in corn samples. Extraction was carried out using MeOH:water (30:70 v/v) solvent at 50°C for 15 min. The on-line SPE-HPLC/UV approach combined reversed solid-phase extraction using strata X sorbent with MeOH:H<sub>2</sub>O (80:20 v/v) at 1 mL min<sup>-1</sup> as eluent for the enrichment of the analytes. C18 monolithic column with acetonitrile:10 mM acetate buffer pH 4 (20:80, v/v) was employed as mobile phase at 2 mL min<sup>-1</sup> flow rate for separation of the compounds before UV detection. Enrichment factors up to 13.4 were achieved with a 10 mL sample volume. The developed procedure showed linear response ranges from 0.07–0.70 mg kg<sup>−1 </sup>for 2,4-D and atrazine with correlation coefficients &gt;0.993. The LODs were 0.03 and 0.02 mg kg<sup>-1 </sup>for 2,4-D and atrazine, respectively with RSD ranged from 4.0 to 7.2 % at 0.07 and 0.30 mg kg<sup>-1</sup>. The recoveries of 2,4-D and atrazine in corn samples were from 82.6 and 98.2%. The proposed method showed good recoveries and reasonable precision for herbicide analysis in corn samples avoiding the time-consuming batch sample pretreatment step, thus minimizing risks of sample contamination and analyte losses.</p>

Multiparameter Optimization of Magnetite Solid-phase Microextraction for Preconcentration of Diclofenac and Determination by UV-Vis Spectrophotometry

2021 ◽  
Author(s):  
Hassan Ali Shahhosseini ◽  
Somayeh Heydari ◽  
Zarrin Es'haghi ◽  
Leili Zare
Keyword(s):  
Solid Phase ◽  
Correlation Coefficients ◽  
Sample Volume ◽  
Effective Parameters ◽  
Dialdehyde Starch ◽  
Main Effect ◽  
Ft Ir ◽  
Multiparameter Optimization ◽  
Optimized Conditions

Abstract This research, aimed to synthesis and functionalize of Fe3O4 magnetic nanoparticles (MNPs) using dialdehyde starch and modifying with arginine amino acid. The resulting MNPs were characterized by Fourier transform infrared spectroscopy (FT-IR), Scanning electron microscope (SEM) and Vibrating sample magnetometer (VSM). Synthesized MNPs were developed for preconcentration and determination of diclofenac in biological samples by UV- Vis Spectrophotometry. A Plackett–Burman experimental design was used to evaluate the influence of effective parameters. Significant parameters were further optimized by Central Composite Design (CCD). Sample volume, pH and salting effect had a main effect on extraction of diclofenac by the proposed method. Under the optimized conditions, the detection limit (3Sb, n = 7) was found to be 0.039 µg ml− 1.The calibration curve showed dynamic linear 0.05-10 µg ml− 1 with correlation coefficients (R2) of 0.987. The enrichment factor was found to be 148. The proposed method showed good results for preconcentration and determination of diclofenac in serum and pharmaceutical samples.

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