Ultrasound-Assisted Ionic Liquid Microextraction for Preconcentration of Cadmium in Water, Vegetables and Hair Samples Prior to FAAS Determination

2020 ◽  
Vol 16 (8) ◽  
pp. 1022-1031
Author(s):  
Eman M. Hafez ◽  
Ragaa El Sheikh ◽  
Ali A. Sayqal ◽  
Najla AlMasoud ◽  
Ayman A. Gouda
Keyword(s):  
Ionic Liquid ◽  
Limit Of Detection ◽  
Certified Reference Materials ◽  
Standard Addition ◽  
Calibration Graph ◽  
Extraction Solvent ◽  
Hair Samples ◽  
Relative Standard ◽  
Living Organisms ◽  
The Impact

Background:: Cadmium (Cd2+) is considered to be one of the most important hazardous heavy metals due to its toxicity for living organisms at low concentration levels. Therefore, the estimation of trace Cd2+ in different types of various samples is a very important objective for chemists using effective methods. In the present work, a novel, green, easy and fast ultrasoundassisted ionic liquid-dispersive liquid phase microextraction technique (UA-IL-DLPME) was developed to preconcentrate and determine trace quantities of cadmium (Cd2+) ions from real samples, prior to detection by FAAS. Methods: The proposed technique is based on utilization of ionic liquid (IL) (1-hexyl-3- methylimidazolium tris(pentafluoroethyl)trifluorophosphate [HMIM][FAP]) as an extraction solvent for Cd2+ ions after complexation with 2-(6-methylbenzothiazolylazo)-6-nitrophenol (MBTANP) at pH 7.0. The impact of different analytical parameters on the microextraction efficiency was investigated. The validation of the proposed procedure was verified by the test of two certified reference materials (TMDA-51.3 fortified water, SRM spinach leaves 1570A) applying the standard addition method. Results: In the range of 2.0-200 μg L−1, the calibration graph was linear. Limit of detection, preconcentration factor and the relative standard deviation (RSD %, 100 μg L-1, n=5) as precision was 0.1 μg L-1, 100 and 3.1%, respectively. Conclusion: Green UA-IL-DLPME method was developed and applied to preconcentrate and determine trace quantities of Cd2+ in real water, vegetables and hair samples with satisfactory results.

scholarly journals A GREEN VORTEX-ASSISTED IONIC LIQUID-BASED DISPERSIVE LIQUID–LIQUID MICROEXTRACTION METHOD FOR PRECONCENTRATION AND DETERMINATION OF TRACE CADMIUM IN FOOD SAMPLES

2019 ◽  
pp. 178-184
Author(s):  
RAGAA EL SHEIKH ◽  
MOHAMMED ABDULLAH ATWA ◽  
AMIRA ATEF ABDULLAH ◽  
ANDAYMAN ABOU ELFETOUH GOUDA
Keyword(s):  
Ionic Liquid ◽  
Limit Of Detection ◽  
Food Samples ◽  
Chromotropic Acid ◽  
Calibration Graph ◽  
Flame Atomic Absorption ◽  
Relative Standard ◽  
Dispersive Liquid Liquid Microextraction ◽  
The Impact ◽  
Liquid Microextraction

Objective: Green, easy, and sensitive vortex-assisted ionic liquid-based dispersive liquid–liquid microextraction technique (VA-IL-DLLME) was developed to preconcentrate and determine trace quantities of cadmium (Cd2+) ions from real food samples, before detection by flame atomic absorption spectrometry. Methods: The proposed technique base on the utilization of IL (1-hexyl-3-methylimidazolium tris(pentafluoroethyl)trifluorophosphate) as an extraction solvent for Cd2+ ions after the complexation with 2-(2’-benzothiazolylazo) chromotropic acid at pH 8.0. The impact of different analytical parameters on microextraction efficiency was investigated. The validation of the proposed procedure was verified by the test of certified reference material (SRM spinach leaves 1570A) applying the standard addition method. Results: In the range of 1.0–300 μg/L, the calibration graph was linear. Limit of detection, preconcentration factor and the relative standard deviation (RSD%, 25, 150, and 250 μg/L, n=5) were 0.2 μg/L, 100, and 2.0–3.2%, respectively. Conclusion: Green, VA-IL-DLLME method was developed and applied to preconcentrate and determine of trace quantities of Cd2+ in real food samples with satisfactory results. The obtained recovery values showed good agreement with the certified values.

GREEN VORTEX-ASSISTED IONIC LIQUID-BASED DISPERSIVE LIQUID-LIQUID MICROEXTRACTION FOR ENRICHMENT AND DETERMINATION OF CADMIUM AND LEAD IN WATER, VEGETABLES AND TOBACCO SAMPLES

2020 ◽  
pp. 103-110
Author(s):  
RAGAA EL-SHEIKH ◽  
WAFAA S. HASSAN ◽  
SARA H. IBRAHIM ◽  
AMIRA M. YOUSSEF ◽  
AYMAN A. GOUDA
Keyword(s):  
Ionic Liquid ◽  
Disodium Salt ◽  
Extraction Solvent ◽  
Relative Standard ◽  
Chromotrope 2R ◽  
Preconcentration Factor ◽  
Dispersive Liquid Liquid Microextraction ◽  
Cadmium And Lead ◽  
The Impact ◽  
Liquid Microextraction

Objective: An eco-friendly, simple and sensitive vortex-assisted ionic liquid-based dispersive liquid-liquid microextraction method (VA-IL-DLLµE) has been proposed to enrich and determine trace levels of cadmium (Cd2+ ) and lead (Pb2+ ) ions in water, vegetables and tobacco samples, prior to its FAAS determination. Methods: The proposed method based on utilization of ionic liquid (IL) (1-hexyl-3-methylimidazolium tris(pentafluoroethyl)trifluorophosphate [HMIM][FAP]) as an extraction solvent for both ions after the complexation with 4,5-dihydroxy-3-phenylazo-2,7-naphthalenedisulfonic acid, disodium salt (Chromotrope 2R) at pH 6.5. The impact of different analytical parameters on microextraction efficiency was optimized. Results: In the ranges of 1.0–300 and 2.0-400 μg/ml, the calibration graphs were linear. The limits of detection were 0.3 and 0.6 μg/ml for Cd2+ and Pb2+ ions, respectively. The preconcentration factor was 100. The relative standard deviation (RSD %)<3.0%, which indicates the proposed method has high precision. Conclusion: The proposed VA-IL-DLLµE method was developed and applied for the estimation of Cd2+ and Pb2+ ion content in various water, vegetables and tobacco samples, and satisfactory results were obtained. The obtained recovery values showed good agreement with the certified values.

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 Determination of cobalt in water samples by atomic absorption spectrometry after pre-concentration with a simple ionic liquid-based dispersive liquid-liquid micro-extraction methodology

2010 ◽  
Vol 8 (3) ◽  
pp. 617-625 ◽  
Author(s):  
Hossein Abdolmohammad-Zadeh ◽  
Elnaz Ebrahimzadeh
Keyword(s):  
Ionic Liquid ◽  
Atomic Absorption Spectrometry ◽  
Atomic Absorption ◽  
Water Samples ◽  
Limit Of Detection ◽  
Absorption Spectrometry ◽  
Experimental Conditions ◽  
Flame Atomic Absorption ◽  
Relative Standard

AbstractA rapid dispersive liquid-liquid micro-extraction (DLLME) methodology based on the application of 1-hexylpyridinium hexafluorophosphate [C6py][PF6] ionic liquid (IL) as an extractant solvent was applied for the pre-concentration of trace levels of cobalt prior to determination by flame atomic absorption spectrometry (FAAS). 1-Phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP) was employed as a chelator forming a Co-PMBP complex to extract cobalt ions from aqueous solution into the fine droplets of [C6py][PF6]. Some effective factors that influence the micro-extraction efficiency include the pH, the PMBP concentration, the amount of ionic liquid, the ionic strength, the temperature and the centrifugation time which were investigated and optimized. In the optimum experimental conditions, the limit of detection (3s) and the enrichment factor were 0.70 µg L−1 and 60, respectively. The relative standard deviation (RSD) for six replicate determinations of 50 µg L−1 Co was 2.36%. The calibration graph using the pre-concentration system was linear at levels 2–166 µg L−1 with a correlation coefficient of 0.9982. The applicability of the proposed method was evaluated by the determination of trace amounts of cobalt in several water samples.

scholarly journals Analysis of the Chloroacetanilide Herbicides in Water Using SPME with CAR/PDMS and GC/ECD

2005 ◽  
Vol 88 (4) ◽  
pp. 1236-1241 ◽  
Author(s):  
Ying-Ming Hwang ◽  
Yih-Gang Wong ◽  
Wu-Hsiung Ho
Keyword(s):  
Humic Acid ◽  
Ph Value ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Standard Addition ◽  
Electron Capture Detection ◽  
Detection Analysis ◽  
Salt Addition ◽  
Chloroacetanilide Herbicides ◽  
Relative Standard

Abstract The solid-phase microextraction (SPME) technique using a 75 mm film of carboxen/polydimethylsiloxane was applied to the analysis of chloroacetanilide herbicides (acetochlor, alachlor, butachlor, metolachlor, and propachlor) residues. The feasibility of SPME with gas chromatography electron capture detection analysis has been evaluated. The effects of experimental parameters such as magnetic stirring, salt addition, humic acid addition, pH value, and extraction time, as well as desorption temperature and time, were investigated. Analytical parameters such as linearity, repeatability and limit of detection were also evaluated. The inhibition of humic acid to the extraction of chloroacetanilide herbicides was observed. A standard addition method for calibration was recommended to reduce deviations caused by matrix interferences. The proposed method provided a simple and rapid analytical procedure for chloroacetanilide herbicides in water with limits of detection 0.002–0.065 μg/L for deionized water, and 0.005–0.22 μg/L for farm water. The relative standard deviations (n = 5) for analyses of farm water were 7–20% for 0.5 μg/L chloroacetanilide herbicides. This application was illustrated by the analysis of sample collected from farm water in the Chung-hwa area, Taiwan.

scholarly journals Determination of carcinogenic herbicides in milk samples using green non-ionic silicone surfactant of cloud point extraction and spectrophotometry

2018 ◽  
Vol 5 (4) ◽  
pp. 171500 ◽  
Author(s):  
N. I. Mohd ◽  
N. N. M. Zain ◽  
M. Raoov ◽  
S. Mohamad
Keyword(s):  
Cloud Point ◽  
Cloud Point Extraction ◽  
Limit Of Detection ◽  
Cost Effective ◽  
Silicone Surfactant ◽  
Extraction Solvent ◽  
Milk Samples ◽  
Relative Standard ◽  
Limit Of Quantitation

A new cloud point methodology was successfully used for the extraction of carcinogenic pesticides in milk samples as a prior step to their determination by spectrophotometry. In this work, non-ionic silicone surfactant, also known as 3-(3-hydroxypropyl-heptatrimethylxyloxane), was chosen as a green extraction solvent because of its structure and properties. The effect of different parameters, such as the type of surfactant, concentration and volume of surfactant, pH, salt, temperature, incubation time and water content on the cloud point extraction of carcinogenic pesticides such as atrazine and propazine, was studied in detail and a set of optimum conditions was established. A good correlation coefficient ( R 2 ) in the range of 0.991–0.997 for all calibration curves was obtained. The limit of detection was 1.06 µg l −1 (atrazine) and 1.22 µg l −1 (propazine), and the limit of quantitation was 3.54 µg l −1 (atrazine) and 4.07 µg l −1 (propazine). Satisfactory recoveries in the range of 81–108% were determined in milk samples at 5 and 1000 µg l −1 , respectively, with low relative standard deviation, n  = 3 of 0.301–7.45% in milk matrices. The proposed method is very convenient, rapid, cost-effective and environmentally friendly for food analysis.

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.

Simultaneous Determination of Four Plant Hormones in Soil by Ultrasound-Assisted Ionic Liquid Based Dispersive Liquid-Liquid Microextraction

2014 ◽  
Vol 675-677 ◽  
pp. 181-184 ◽  
Author(s):  
Gui Qi Huang ◽  
She Ying Dong ◽  
Zhen Yang ◽  
Ting Lin Huang
Keyword(s):  
Ionic Liquid ◽  
Plant Hormones ◽  
High Performance ◽  
Extraction Solvent ◽  
Target Analytes ◽  
Relative Standard ◽  
Ultrasound Assisted ◽  
Dispersive Liquid Liquid Microextraction ◽  
Liquid Microextraction

An ultrasound-assisted ionic liquid based dispersive liquid-liquid microextraction (UA-IL-DLLME) was developed for the determination of four plant hormones (6-benzyladenine (6-BA), kinetin (6-KT), 2, 4-dichlorophenoxy acetic acid (2, 4-D) and uniconazole (UN)) in soil, using high performance liquid chromatography (HPLC)-diode array detection (DAD). Several important parameters including the type and volume of extraction solvent, the volume of disperser solvent, ultrasound time, pH of the solution and salt effect were studied and optimized. Under optimum conditions, the limits of detections (LODs) for the target analytes were in the range of 0.002-0.01 μg g-1. And satisfactory recoveries of the target analytes in the soil samples were 79.3-96.7 %, with relative standard deviations (RSD, n=5) that ranged from 4.3 to 6.7%.

scholarly journals Sensitive Determination of Terazosin in Pharmaceutical Formulations and Biological Samples by Ionic-Liquid Microextraction Prior to Spectrofluorimetry

2012 ◽  
Vol 2012 ◽  
pp. 1-7 ◽  
Author(s):  
Mohsen Zeeb ◽  
Mahdi Sadeghi
Keyword(s):  
Ionic Liquid ◽  
Ionic Strength ◽  
Biological Samples ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Experimental Conditions ◽  
Relative Standard ◽  
Common Ion ◽  
Liquid Microextraction

An efficient and environmentally friendly sample preparation method based on the application of hydrophobic 1-Hexylpyridinium hexafluorophosphate [Hpy][PF6] ionic liquid (IL) as a microextraction solvent was proposed to preconcentrate terazosin. The performance of the microextraction method was improved by introducing a common ion of pyridinium IL into the sample solution. Due to the presence of the common ion, the solubility of IL significantly decreased. As a result, the phase separation successfully occurred even at high ionic strength, and the volume of the settled IL-phase was not influenced by variations in the ionic strength (up to 30% w/v). After preconcentration step, the enriched phase was introduced to the spectrofluorimeter for the determination of terazosin. The obtained results revealed that this system did not suffer from the limitations of that in conventional ionic-liquid microextraction. Under optimum experimental conditions, the proposed method provided a limit of detection (LOD) of 0.027 μg L−1and a relative standard deviation (R.S.D.) of 2.4%. The present method was successfully applied to terazosin determination in actual pharmaceutical formulations and biological samples. Considering the large variety of ionic liquids, the proposed microextraction method earns many merits, and will present a wide application in the future.

Determination of diltiazem based on the reduction of Cu(II)–BCA complexes in micellar medium

2010 ◽  
Vol 88 (6) ◽  
pp. 533-539 ◽  
Author(s):  
Larissa Zuppardo Lacerda Sabino ◽  
Daniele Cestari Marino ◽  
Horacio Dorigan Moya
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Confidence Level ◽  
Limit Of Detection ◽  
Calibration Graph ◽  
Micellar Medium ◽  
Solution Ph ◽  
Simple Method ◽  
Relative Standard

A simple method was developed for determining microquantities of diltiazem, based on the reduction of copper(II) in buffered solution (pH 7.0) and the use of a micellar medium containing 4,4′-dicarboxy-2,2′-biquinoline acid. The copper(I) produced reacts with 4,4′-dicarboxy-2,2′-biquinoline acid and the complexes formed are spectrophotometrically measured at 558 nm. A typical calibration graph shows good linearity (r = 0.993) from 20 to 100 μg mL–1 of diltiazem. The limit of detection and relative standard deviation were calculated as 12 μg mL–1 (99% confidence level) and 3.5% (40 μg mL–1; n = 6), respectively, with a mean recovery value of 96.5% found in pharmaceutical dosages. A straightforward and effective way to recycle the reagents is addressed. The hazardous aspects of the Cu(I)–BCA reaction are presented as well.

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