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 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 New sporopollenin-based β-cyclodextrin functionalized magnetic hybrid adsorbent for magnetic solid-phase extraction of nonsteroidal anti-inflammatory drugs from water samples

2018 ◽  
Vol 5 (7) ◽  
pp. 171311 ◽  
Author(s):  
Syed Fariq Fathullah Syed Yaacob ◽  
Muhammad Afzal Kamboh ◽  
Wan Aini Wan Ibrahim ◽  
Sharifah Mohamad
Keyword(s):  
Solid Phase Extraction ◽  
Water Samples ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Magnetic Solid Phase Extraction ◽  
Phase Extraction ◽  
Relative Standard ◽  
Magnetic Solid ◽  
Inflammatory Drugs ◽  
Anti Inflammatory

A magnetic solid-phase extraction (MSPE) procedure on the newly synthesized magnetic β-cyclodextrin functionalized with toluene diisocyanate (TDI) as a linker and further modified with bio-polymeric spores of sporopollenin (MSp-TDI-βCD), was developed for the extraction of nonsteroidal anti-inflammatory drugs (NSAIDs), namely, indoprofen (INP), ketoprofen (KTP), ibuprofen (IBP) and fenoprofen (FNP) from water samples prior to their HPLC-DAD determination. The newly synthesized MSp-TDI-βCD was comprehensibly characterized using FT-IR, XRD, SEM-EDX, BET and VSM analyses. The separation of selected NSAIDs on MSp-TDI-βCD from aqueous solution was simply achieved by applying an external magnetic field via a permanent magnet. The MSPE parameters affecting extraction performance, i.e. sorbent dosage, sample volume, extraction and desorption time, type of organic eluent and volume and solution pH were investigated and optimized. The proposed method showed linear range between 0.5 and 500 ng ml −1 , low limit of detection at S/N = 3 (0.16–0.37 ng ml −1 ) and limit of quantification at S/N = 10 (0.53–1.22 ng ml −1 ). The inter-day ( n =  15) and intra-day ( n =  5) precision for the proposed methods given by relative standard deviation (RSD%) was in the range of 2.5–4.0 and 2.1–5.5, respectively. The extraction recoveries of NSAIDs from environmental samples (tap, drinking and river water) ranged from 92.5% to 123.6%, with satisfactory precision (RSD% less than 12.4%).

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%).

scholarly journals Application of micro-nanostructured magnetite in separating tetrabromobisphenol A and hexabromocyclododecane from environmental water by magnetic solid phase extraction

PLoS ONE ◽  
2021 ◽  
Vol 16 (5) ◽  
pp. e0251021
Author(s):  
Xiaoping Wang ◽  
Fengzhi He ◽  
Limin Zhang ◽  
Ang Yu
Keyword(s):  
Solid Phase Extraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Magnetic Solid Phase Extraction ◽  
Environmental Water ◽  
Mass Spectrometry Analysis ◽  
Tetrabromobisphenol A ◽  
Phase Extraction ◽  
Relative Standard ◽  
Magnetic Solid

Two typical brominated flame retardants (BFRs), namely, tetrabromobisphenol A (TBBPA) and hexabromocyclododecane (HBCD), were persistent organic pollutants widely detected in various environmental media. This study aimed to successfully synthesize micro-nano-structured magnetite particles (MNMPs) with surface modification by citric acid molecules. The synthesized composites served as an adsorbent for extracting TBBPA and HBCD from environmental water samples followed by gas chromatography–mass spectrometry analysis. The obtained MNMPs were characterized in terms of crystal structure, morphology, size distribution, hydrophobic and hydrophilic performance and magnetism. The results indicated that the MNMPs exhibited high surface area, good dispersibility, and strong magnetic responsiveness for separation. The parameters affecting the extraction efficiency were optimized, including sample pH, amount of sorbents, extraction time and desorption conditions. Under the optimum conditions, the recovery was 83.5 and 107.1%, limit of detection was 0.13 and 0.35μg/mL (S/N = 3), and limit of quantification was 0.37 and 0.59 μg/mL (S/N = 10) for TBBPA and HBCD respectively. The relative standard deviations obtained using the proposed method were less than 8.7%, indicating that the MNMP magnetic solid-phase extraction method had advantages of simplicity, good sensitivity and high efficiency for the extraction of the two BFRs from environmental water.

scholarly journals Preparation of Polyphenol-Coated CoFe2O3 Nanoparticles for Magnetic Solid-Phase Extraction and Preconcentration of Lawsone by High-Performance Liquid Chromatography – DAD

2020 ◽  
Author(s):  
Hassan Arkaban ◽  
Mohammad Mirzaei ◽  
Mansoreh Behzadi
Keyword(s):  
Solid Phase Extraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Oxidative Polymerization ◽  
Magnetic Solid Phase Extraction ◽  
Polymerization Process ◽  
Phase Extraction ◽  
Extraction Temperature ◽  
Relative Standard ◽  
Magnetic Solid

A novel polyphenol‑coated CoFe2O4 system was synthesized as a magnetic adsorbent by chemical oxidative polymerization process for magnetic solid-phase extraction of lawsone. The synthesized nanoadsorbent showed a spherical morphology with diameters under 50 nm by scanning electron microscopy images. The extraction efficiency of this adsorbent was studied towards the extraction of lawsone from saline aqueous solution in dispersion mode. Major parameters including the type and volume of desorption solvent, amount of sorbent, desorption time, extraction time, extraction temperature, ionic strength and pH were optimized. Under the optimum conditions the relative standard deviation in 0.005 µg mL-1 (inter-day n = 6; intra-day: n = 6; and adsorbent to adsorbent n = 4) were obtained as 5.2, 8.07 and 11.7%, respectively. A linear calibration curve in the range of 0.003–0.5 µg mL-1 with R2 = 0.993 was obtained. The limit of detection and limit of quantification of the method were 0.001 µg mL-1 and 0.003 µg mL-1, respectively. The relative recovery percentages were in range of 90-96.4% for henna leaves, henna shampoo, and henna dermal lotion real 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.

Detecting PAEs in Bottled Water by SPE-LC/QQQ

2013 ◽  
Vol 469 ◽  
pp. 444-449
Author(s):  
Yu Zi Liu ◽  
Ying Hao Xing ◽  
Jun Wu
Keyword(s):  
Drinking Water ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
Bottled Water ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
The Common ◽  
Acid Esters

In this study, High Performance Liquid Chromatography (HPLC), combined with Triple Quadruple mass Spectrometry (QQQ) were developed and applied in the analysis of 16 phthalic acid esters (PAEs) in the common drinking water. Qualitative and quantitative analysis were carried out by Multiple Reaction Monitoring (MRM). The method, combined with Solid Phase Extraction, was established to detect the PAEs in drinking water. As showed by the results, 16 PAEs had a good linearity in the range of 1.14~101.4μg/L, with correlation coefficient between 0.996~0.999. The mean recoveries were in the range of 87.53~131.37%, with the relative standard deviation be 0.71~5.09%. The limit of quantification (LOQ) of 16 PAEs were between 1.14~32.51μg/L, with the limit of detection (LOD) be 0.34~10.67μg/L. There were five PAEs which were detected in the range of <1.7~17.2μg/L in bottled water. Some products have some PAEs which havent been shown in the national or the international standard of the drinking water.

scholarly journals Extraction and Determination of Oxymatrine Pesticide in Environmental Sample and in its Formulation using High-Performance Liquid Chromatography

2020 ◽  
Vol 8 (2) ◽  
pp. 1-7
Author(s):  
Ihsan M. Shaheed ◽  
Saadiyah A. Dhahir
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Water Samples ◽  
High Performance ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Relative Standard ◽  
Dispersive Liquid Liquid Microextraction

The quinolizindine alkaloid compound, oxymatrine pesticide, was analysis in the river water samples collected from different agriculture areas in the Iraqi city of Kerbala and also in its formulation using developed reverse-phase high-performance liquid chromatography method. Acetonitrile:methanol (60:40 v/v) was chosen as mobile phase at pH (7.0), flow rate 0.5 mL/min, and 20 µL as volume injection. Modified ecological-friendly method, dispersive liquid-liquid microextraction, was used for the extraction of oxymatrine from water samples. Linearity study was constructed from 0.1 to 70 μg/mL at λmax 205 nm. The limit of detection and limit of quantification were 0.025 and 0.082 μg/mL, respectively, and the relative standard deviation (RSD) % was 0.518%. Three spiked levels of concentration (20.0, 40.0, and 70.0 μg/mL) were used for the validation method. The percentage recovery for the three spiked samples was ranged between 98.743 and 99.432 and the RSD% was between 0.051 and 0.202%, the formulation studies of oxymatrine between 99.487 and 99.798, and the RSD% was ranged from 0.045 to 0.057%. The developed method can be used accurately and selectively for the determination of oxymatrine in environmental samples and in the formulation.

scholarly journals Analytical method validation of reversed phase HPLC for quantitative analysis of tartrazine and auramine o in powder drinks

Food Research ◽  
2020 ◽  
Vol 4 (6) ◽  
pp. 2037-2041
Author(s):  
A.D. Lestari ◽  
A. Rohman ◽  
S. Martono
Keyword(s):  
Method Validation ◽  
Analytical Method ◽  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Coefficient Of Determination ◽  
Array Detector ◽  
Analytical Method Validation ◽  
Relative Standard ◽  
Auramine O

This study was aimed to perform analytical method validation of high-performance liquid chromatography (HPLC) technique using photo-diode array detector for the simultaneous determination of Tartrazine (TAR) and Auramine O (AUO) in powder drink products. TAR and AUO were analysed using Waters Shield C18 column (250 mm x 4.6 mm i.d., 5 µm) using PDA detector at 300-650 nm. The mobile phase used was acetonitrileammonium acetate 19 mM (86:14 v/v) delivered isocratically at a flow rate of 1.2 mL/ min. The optimized HPLC condition was subjected to analytical method validation by assessing some performance characteristics as guided by International Conference on Harmonization (ICH). The method was linear over the studied concentration ranges with the coefficient of determination (R2 ) of 0.999 and 0.997 for TAR and AUR with % intercept less than 2%, respectively. The developed method was sensitive with a limit of detection value of 0.0325 μg/mL and 0.1052 μg/mL for TAR and AUO, respectively. The method is also accurate and precise as indicated with acceptable recovery values of 99.0- 100.7% for TAR and 102.1-106.5% for AUO with relative standard deviation (RSD) values lower than those required by Association of Official Analytical Chemists’ (AOAC). The developed method is simple and can be used for routine analysis of TAR and AUO for quality assurance purposes of powder drinks.

scholarly journals EXTRACTION AND DETERMINATION OF TEBUCONAZOLE IN ENVIRONMENTAL SAMPLES FROM THE CITY OF KERBALA, IRAQ AND IN ITS FORMULATION USING HIGH- PERFORMANCE LIQUID CHROMATOGRAPHY (HPLC)

2020 ◽  
Vol 17 (34) ◽  
pp. 1046-1054
Author(s):  
Ihsan Mahdi SHAHEED ◽  
Saadiyah Ahmed DHAHIR
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Water Samples ◽  
High Performance ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Percentage Recovery ◽  
Relative Standard

The triazole, tebuconazole pesticide, was determined in its formulation and also in the river water samples collected from different agriculture areas in the Iraqui city of Kerbala using developed high-performance liquid chromatography method(HPLC) with UV-visible detection, The mobile composition phase was a mixture of acetonitrile:methanol (50:50 v/v) and the column was C18 (250 cm x 4.6 mm,5μm). Also modified dispersive liquidliquid microextraction (DLLME), which is regarded as an ecological -friendly method, was used for the extraction of tebuconazole from water samples using acetonitrile and chloroform as solvents extraction and dispersive agent, respectively. Linearity to maintain the calibration curve was achieved from (0.1-70) μg.mL-1 with a limit of detection(0.053) μg.mL-1 and limit of quantification (0.174) μg.mL-1. Three spiked levels of concentration (1.0, 5.0, and 10) μg.mL-1 were used for the validation of the method. The relative standard deviation (RSD%) was (0.294- 0.813)%, and the percentage recovery was (100.001-100.005). The formulation studies for two different concentrations (10 and 40) μg.mL-1, which prepared from tebuconazole formulation (Raxil ODS2 2%), gave acceptable percentage recovery between (98.956-99.833). The developed method can be used accurately for the determination of tebuconazole in water samples and in the formulation of tebuconazole effectively.

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