Adsorption of Organic Pollutants in Wastewater using Solid Phase Extraction Absorbent from Agro-Waste

2019 ◽  
Vol 7 (2) ◽  
pp. 245-253 ◽  
Author(s):  
Wan Norfazilah Wan Ismail ◽  
Dzul Iskandar Muhammad Fauzi ◽  
Nurlin Abu Samah
Keyword(s):  
Solid Phase Extraction ◽  
Organic Pollutants ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Sample Volume ◽  
Wastewater Sample ◽  
Phase Extraction ◽  
Nano Powder ◽  
Optimum Parameters ◽  
Limit Of Quantitation

A rapid solid phase extraction (SPE) combined with gas chromatography equipped with mass spectrometry (GC-MS) method was developed and validated for the determination of acenaphthylene, acenaphthene and naphthalene in wastewater sample collected from petroleum industry’s drainage. Important SPE parameters, namely absorbent amount, sample volume, type of elution solvent and its volume were optimized. The optimum parameters obtained are: 200 mg silica nano-powder, 2.0 mL sample volume and 2.0 mL n-hexane as elution solvent. The method showed good linearity in the range of 0.1-10.0 mg/L with satisfactory limit of detection (≤1.0 mg/L) and limit of quantitation (≤3.2 mg/L) under the optimized conditions. Good relative recoveries (94.7-99.9%) and intra- and inter-day precisions (≤2.8%, n=3) for acenaphthene, acenaphthylene and naphthalene were obtained. Toxicity study has revealed that it is a non-toxic absorbent and safe to be used for the removal of organic pollutants in water which is advantageous for routine wastewater analysis.

scholarly journals Development and Validation of RP-HPLC Method for Azilsartan Medoxomil Potassium Quantitation in Human Plasma by Solid Phase Extraction Procedure

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Paras P. Vekariya ◽  
Hitendra S. Joshi
Keyword(s):  
Solid Phase Extraction ◽  
Human Plasma ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Phase Extraction ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
Azilsartan Medoxomil

Simple and rapid reverse phase high-performance liquid chromatography (RP-HPLC) method was developed and validated using solid phase extraction (SPE) technique for the determination of Azilsartan Medoxomil Potassium (AMP) in human plasma; detection was carried out by photo diode array detector. Chromatographic separation of the analyte AMP was achieved within 7.5 min by Waters symmetry C18 (4.6 × 250 mm, 5 µm) column, mobile phase was 25 mM ammonium acetate buffer (pH 5.5): acetonitrile 55 : 45 v/v, flow rate was 1.0 mL/min, and the detection was carried out at 254 nm. Calibration curve was linear (r2 > 0.9985) in the range of 1.0–9.0 µg/mL, limit of detection (LOD) and limit of quantitation (LOQ) were 0.150 µg/mL and 0.400 µg/mL, respectively, and intra- and interday deviations were between 1.53–8.41% and 1.78–4.59%, respectively. The overall mean recovery of AMP was 92.35%. No any endogenous constituents were found to interfere at retention time of the analyte. This new RP-HPLC method was successfully validated and may be applied to conduct bioavailability and bioequivalence studies of AMP.

Quantitation of 1α,25-dihydroxyvitamin D by LC-MS/MS using solid-phase extraction and fixed-charge derivitization in comparison to immunoextraction

2015 ◽  
Vol 53 (9) ◽  
Author(s):  
Nancy Chan ◽  
Erin J. Kaleta
Keyword(s):  
Solid Phase Extraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Fixed Charge ◽  
Reference Laboratory ◽  
Phase Extraction ◽  
Dihydroxyvitamin D ◽  
Limit Of Quantitation ◽  
Attractive Option ◽  
Assay Precision

AbstractThe objective of this study was to present analysis of 1α,25-dihydroxyvitamin D (DHVD) by solid-phase extraction (SPE) using fixed-charge derivitization extraction to enhance ionization for liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) in comparison to traditional immunoextraction (IE) techniques.Full analytical validation of both a SPE and IE LC-MS/MS assay was performed, and included accuracy, intra- and inter-assay precision, limit of detection and limit of quantitation. Performance of these two assays was compared with reference laboratory IE LC-MS/MS testing.This SPE LC-MS/MS assay demonstrated similar performance to the IE LC-MS/MS assay validated simultaneously. Intra-assay precision for low (12 pg/mL), medium (25 pg/mL) and high (60 pg/mL) control samples was 7.2%, 13.7% and 11.3% for DHVD2, respectively, and 9.1%, 5.9% and 8.9% for DHVD3. The inter-assay precision was 11.6%, 10.3% and 3.9% for DHVD2 and 10.6%, 7.0% and 5.6% for DHVD3. The limit of detection was 1.9 and 2.7 pg/mL for DHVD2 and DHVD3, and limit of quantitation was 4 pg/mL for both DHVD2 and DHVD3. Comparison to a reference LC-MS/MS assay showed excellent correlation (slope 0.936, RThe study demonstrated comparability of the SPE-LC-MS/MS assay for analysis of DHVD and offers an attractive option for assessment of vitamin D status as an alternative to traditional IE techniques.

scholarly journals Survey of Octylphenol, Nonylphenol, and Bisphenol A in Infant Milk Powders by Solid-Phase Extraction Combined GC/MS Method

2018 ◽  
Vol 2018 ◽  
pp. 1-8
Author(s):  
Chenggang Cai ◽  
Yibin Ying ◽  
Pinggu Wu ◽  
Jun Tang ◽  
Liyuan Wang ◽  
...  
Keyword(s):  
Bisphenol A ◽  
Solid Phase Extraction ◽  
Endocrine Disruptors ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Milk Powder ◽  
Phase Extraction ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Infant Milk Powder

A detection method for 3 kinds of phenolic compounds of endocrine disruptors (4-nonylphenol, 4-octylphenol, and bisphenol A) in infant milk powders by solid-phase extraction combined GC-MS was established. This method can effectively remove interference materials from infant milk powder products. The limit of detection and the limit of quantitation of the 3 kinds of compounds were 0.8 μg/kg and 2.5 μg/kg, respectively, with the relative standard deviations of 4.3–12.1%. The recovery rates of 4-nonylphenol, 4-octylphenol, and bisphenol A were of 68.5–89.2%, 64.8–87.0%, and 97.8–110.0%, respectively. Concentrations of the bisphenol A were from 0.8 to 14 μg/kg in 35 samples of the total 60 samples. And the other two compounds of 4-nonylphenol and 4-octylphenol were not found in all the 60 samples tested. The established method is simple, rapid, accurate, and highly sensitive, and the pollution of endocrine disruptors in some infant milk powders products was detectable in trace amounts.

scholarly journals Performance comparison between solid phase extraction and magnetic carbon nanotubes facilitated dispersive-micro solid phase extractions (Mag-CNTs/d-µSPE) of a cyanide metabolite in biological samples using GC–MS

2021 ◽  
Vol 12 (1) ◽  
Author(s):  
Sun Yi Li ◽  
Ilona Petrikovics ◽  
Jorn Yu
Keyword(s):  
Carbon Nanotubes ◽  
Solid Phase Extraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Phase Extraction ◽  
Bovine Blood ◽  
Limit Of Quantitation ◽  
One Step ◽  
Magnetic Carbon ◽  
Magnetic Carbon Nanotubes

AbstractDispersive-micro solid phase extraction (d-µSPE) has gained increasing attention due to its convenience, effectiveness, and flexibility for sorbent selection. Among a various selection of materials, magnetic carbon nanotubes (Mag-CNTs) is a promising d-µSPE sorbent with excellent separation efficiency in addition to its high surface area and adsorption capability. In this work, two different surface-modified Mag-CNTs, Mag-CNTs-COOH and Mag-CNTs-SO3H, were developed to facilitate d-µSPE (Mag-CNTs/d-µSPE). The cyanide metabolite, 2-aminothiazoline-4-carboxylic acid (ATCA), was selected to evaluate their extraction performance using gas chromatography–mass spectrometry (GC–MS) analysis. The Mag-CNTs-COOH enabled a one-step derivatization/desorption approach in the workflow; therefore, a better overall performance was achieved. Compared to the Mag-CNTs-SO3H/d-µSPE and SPE workflow, the one-step desorption/derivatization approach improved the overall extraction efficiency and reduced solvent consumption and waste production. Both Mag-CNTs/d-µSPE workflows were validated according to ANSI/ASB 036 guidelines and showed excellent analytical performances. The limit of detection (LOD) and limit of quantitation (LOQ) of ATCA in synthetic urine were 5 and 10 ng/mL, respectively, and that in bovine blood were achieved at 10 and 60 ng/mL. The SPE method’s LOD and LOQ were also determined at 1 and 25 ng/mL in bovine blood samples. The Mag-CNTs/d-µSPE methods demonstrated great potential to extract polar and ionic metabolites from biological matrices. The extraction processes of ATCA described in this work can provide an easier-to-adopt procedure for potential routine forensic testing of the stable biomarker in cyanide poisoning cases, particularly for those cases where the cyanide detection window has passed.

Development of a solid-phase extraction – spectrofluorimetric method for trace glutathione determination

2011 ◽  
Vol 89 (4) ◽  
pp. 517-523 ◽  
Author(s):  
Ke-Jing Huang ◽  
Cong-Hui Han ◽  
Ying-Ying Wu ◽  
Chao-Qun Han ◽  
De-Jun Niu ◽  
...  
Keyword(s):  
Solid Phase Extraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Signal To Noise Ratio ◽  
Calibration Graph ◽  
Extraction Column ◽  
Phase Extraction ◽  
Selective Reaction ◽  
Spectrofluorimetric Method ◽  
Relative Standard

A simple and efficient solid-phase extraction – spectrofluorimetric method has been developed to determine glutathione (GSH). Fluorescent probe N-(4,4-difluoro-5,7-dimethyl-4-bora-3a,4a-diaza-s-indacene-3-yl)methyl)iodoacetamide (BODIPY Fl-C1-IA) was used as the derivatization reagent. The procedure was based on a BODIPY Fl-C1-IA selective reaction with GSH to form the highly fluorescent product BODIPY Fl-C1-IA–GSH, using a solid-phase extraction column and spectrofluorimetric determination. The variables affecting analytical performance were studied and optimized. The calibration graph using the preconcentration system for GSH was linear over the range of 1–200 nmol/L with a limit of detection of 0.05 nmol/L (signal-to-noise ratio = 3). The relative standard deviation for six replicate determinations of GSH at the 100 nmol/L concentration level was 3.9%. The method was applied to water samples and average recoveries between 87.5% and 111.5% were obtained for spiked samples.

scholarly journals Greener Monolithic Solid Phase Extraction Biosorbent Based on Calcium Cross-Linked Starch Cryogel Composite Graphene Oxide Nanoparticles for Benzo(a)pyrene Analysis

Molecules ◽  
2021 ◽  
Vol 26 (20) ◽  
pp. 6163
Author(s):  
Aree Choodum ◽  
Nareumon Lamthornkit ◽  
Chanita Boonkanon ◽  
Tarawee Taweekarn ◽  
Kharittha Phatthanawiwat ◽  
...  
Keyword(s):  
Graphene Oxide ◽  
Solid Phase Extraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
High Sensitivity ◽  
Rice Flour ◽  
Oxide Nanoparticles ◽  
Phase Extraction ◽  
Limit Of Quantification ◽  
Significant Difference

Benzo(a)pyrene (BaP) has been recognized as a marker for the detection of carcinogenic polycyclic aromatic hydrocarbons. In this work, a novel monolithic solid-phase extraction (SPE) sorbent based on graphene oxide nanoparticles (GO) in starch-based cryogel composite (GO-Cry) was successfully prepared for BaP analysis. Rice flour and tapioca starch (gel precursors) were gelatinized in limewater (cross-linker) under alkaline conditions before addition of GO (filler) that can increase the ability to extract BaP up to 2.6-fold. BaP analysis had a linear range of 10 to 1000 µgL−1 with good linearity (R2 = 0.9971) and high sensitivity (4.1 ± 0.1 a.u./(µgL−1)). The limit of detection and limit of quantification were 4.21 ± 0.06 and 14.04 ± 0.19 µgL−1, respectively, with excellent precision (0.17 to 2.45%RSD). The accuracy in terms of recovery from spiked samples was in the range of 84 to 110% with no significant difference to a C18 cartridge. GO-Cry can be reproducibly prepared with 2.8%RSD from 4 lots and can be reused at least 10 times, which not only helps reduce the analysis costs (~0.41USD per analysis), but also reduces the resultant waste to the environment.

scholarly journals In Situ Miniaturised Solid Phase Extraction (m-SPE) for Organic Pollutants in Seawater Samples

2018 ◽  
Vol 2018 ◽  
pp. 1-6 ◽  
Author(s):  
B. Abaroa-Pérez ◽  
G. Sánchez-Almeida ◽  
J. J. Hernández-Brito ◽  
D. Vega-Moreno
Keyword(s):  
Solid Phase Extraction ◽  
Organic Pollutants ◽  
Marine Environment ◽  
Persistent Organic Pollutants ◽  
Solid Phase ◽  
In Situ Monitoring ◽  
Phase Extraction ◽  
Polycyclic Aromatic ◽  
Seawater Samples

Solid phase extraction (SPE) is a consolidated technique for determining pollutants in seawater samples. The current tendency is to miniaturise systems that extract and determine pollutants in the environment, reducing the use of organic solvents, while maintaining the quality in the extraction and preconcentration. On the other hand, there is a need to develop new extraction systems that can be fitted to in situ continual monitoring buoys, especially for the marine environment. This work has developed a first model of a low-pressure micro-SPE (m-SPE) for persistent organic pollutants (POPs) that can be simply applied to in situ monitoring in the marine environment. This system reduces the volumes of sample and solvents required in the laboratory in comparison with conventional SPE. In the future, it could be used in automated or robotic systems in marine technologies such as marine gliders and oceanographic buoys. This system has been optimised and validated to determine polycyclic aromatic hydrocarbons (PAH) in seawater samples, but it could also be applied to other kinds of persistent organic pollutants (POPs) and emerging pollutants.

scholarly journals Magnetically responsive materials for solid phase extraction

2019 ◽  
Vol 6 (1) ◽  
pp. 15-20 ◽  
Author(s):  
Ivo Safarik ◽  
Jitka Prochazkova ◽  
Eva Baldikova ◽  
Kristyna Pospiskova
Keyword(s):  
Solid Phase Extraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Analytical Techniques ◽  
Magnetic Solid Phase Extraction ◽  
Short Review ◽  
Biologically Active ◽  
Phase Extraction ◽  
Responsive Materials ◽  
Magnetic Solid

Magnetically responsive materials have found many important applications in analytical chemistry. In this short review the basic information about Magnetic solid phase extraction and Magnetic textile solid phase extraction is given. These analytical techniques enable to preconcentrate target biologically active compounds or pollutants from water samples. Both procedures enable to lower the limit of detection using conventional analytical procedures.

scholarly journals Spectrophotometric Determination of Iron(II) after Solid Phase Extraction of Its 2,2′ Bipyridine Complex on Silica Gel-Polyethylene Glycol

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Nahid Pourreza ◽  
Saadat Rastegarzadeh ◽  
Ali Reza Kiasat ◽  
Hossein Yahyavi
Keyword(s):  
Polyethylene Glycol ◽  
Solid Phase Extraction ◽  
Silica Gel ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Extraction Procedure ◽  
Calibration Graph ◽  
Phase Extraction ◽  
Relative Standard

A new solid phase extraction procedure was developed for preconcentration of iron(II) using silica gel-polyethylene glycol (silica-PEG) as an adsorbent. The method is based on retention of iron(II) as 2,2′ bipyridine complex on silica-PEG. The retained complex is eluted by 1.0 mol L−1of sulfuric acid-acetone mixture (1:2) and its absorbance is measured at 518 nm, spectrophotometrically. The effects of different parameters such as pH, concentration of the reagent, eluting reagent, sample volume, amount of adsorbent, and interfering ions were investigated. The calibration graph was linear in the range of 1–60 ng mL−1of iron(II). The limit of detection based on3Sbwas 0.57 ng mL−1and relative standard deviations (R.S.D) for ten replicate measurements of 12 and 42 ng mL−1of iron(II) were 2.4 and 1.7%, respectively. The method was applied to the determination of of iron(II) in water, multivitamin tablet, and spinach samples.

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