In this study, a fast, simple and efficient ultrasound-assisted emulsification microextraction (USAEME) method was successfully developed based on applying low density organic solvents. Fourteen ...microliters of toluene was injected slowly into a 12
mL home-designed centrifuge glass vial containing an aqueous sample that was located inside the ultrasonic water bath. The formed emulsion was centrifuged and 2
μL of separated toluene (about 4
μL) was injected into a gas chromatographic system equipped with a flame ionization detector (GC-FID) for analysis. Some polycyclic aromatic hydrocarbons (PAHs) were selected as model compounds for developing the method and evaluating its performance and to compare the efficiency of the proposed method with previously reported techniques. Several factors influencing the emulsification, extraction and collection efficiency such as the nature and volume of organic solvent, emulsification–extraction temperature, ionic strength and equilibrium and centrifugation times were investigated and optimized. Under the optimum conditions, preconcentration factors (PFs) in a range of 1776–2714 were obtained. The performance of the proposed method was studied in terms of linear dynamic range (LDRs from 0.05 to 100
μg
L
−1), linearity (
R
2
≥
0.994), precision (repeatability: RSD%
≤
7.9, reproducibility: RSD%
≤
14.6) and extraction percents (59.2–90.5%). Limits of detection (LODs) in the range of 0.02–0.05
μg
L
−1 were obtained for different PAHs. The applicability of the proposed method was evaluated by the extraction and determination of PAHs from several natural water samples.
Full text
Available for:
GEOZS, IJS, IMTLJ, KILJ, KISLJ, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UL, UM, UPCLJ, UPUK
The presented study investigates application of decanoic acid-coated Fe
3O
4 nanoparticles as an adsorbent for solid phase extraction and determination of trace amounts of Cd, Co, Cr, Ni, Pb and Zn ...from environmental water samples using flow injection inductively coupled plasma-optical emission spectrometry (ICP-OES). Magnetic nanoparticles (MNPs), carrying target metals, were easily separated from the aqueous solution by applying an external magnetic field; so, no filtration or centrifugation was necessary. After extraction and collection of MNPs, the analytes were desorbed using 0.25
mol
L
−1 of HCl in propanol. The desorbed analytes were introduced into the nebulizer of ICP-OES by using flow injection technique. Effects of pH, chelating agent, extraction time, type of eluent, desorption time and interfering ions on extraction efficiency of the metal ions were investigated and optimized. Under the optimized conditions, detection limits for Cd, Co, Cr, Ni, Pb and Zn were 0.3, 0.7, 0.5, 0.6, 0.8 and 0.2
μg
L
−1, respectively. The enhancement factors of the proposed method for the target metal ions were in the range of 116–150, and the relative standard deviations (RSDs,
C
=
100
μg
L
−1,
n
=
6) were less than 3.5%. The method had a linear dynamic range within the range of 1–400
μg
L
−1. Accuracy of the method was evaluated by recovery measurements on the spiked samples, and good recoveries (92–107%) with low RSDs were achieved.
Full text
Available for:
GEOZS, IJS, IMTLJ, KILJ, KISLJ, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UL, UM, UPCLJ, UPUK
In this study, concentrations of Aluminum (Al), Iron (Fe), Chromium (Cr), Copper (Cu), Nickel (Ni), Vanadium (V), Zinc (Zn), Arsenic (As), Cobalt (Co) and lead (Pb) in the surface sediments from ...Chabahar Bay were studied to assess the degree of heavy metal pollution as a consequence of natural and anthropogenic sources. Metal contents in the sediments were observed in the order of: Al>Fe>Cr>V>Ni>Zn>Cu>>As>Pb>Co. According to enrichment factor (EF), Arsenic was higher than 1.5 at some sites, indicating anthropogenic inputs. Contents of Ni, As and Cr in the some sampling sites were higher than sediment quality guideline implying adverse impacts of these metals. Based on potential ecological risk (PER), the Chabahar Bay had low ecological risk.
•Metals and major elements were determined in surface sediments from Chabahar Bay, Oman Sea.•EF values indicated non-enriched to moderate-enriched.•Ni, As and Cr were above ERL values.
Full text
Available for:
GEOZS, IJS, IMTLJ, KILJ, KISLJ, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UL, UM, UPCLJ, UPUK, ZRSKP
•DCF-EME method for preconcentration of six OCPs in seawater samples was developed.•Effervescence induced by ultrasound radiations was applied for phase separation.•In DCF-EME method more precise and ...effective solvent collection can be achievable.•A home-made extraction cell was design for facile retrieving of solvents.•Analysis of samples collected from Caspian Sea was done.
Dissolved carbon dioxide flotation after emulsification microextraction (DCF-EME) technique coupled with gas chromatography-electron capture detection (GC-ECD) was introduced for preconcentration and determination of six organochlorine pesticides (OCPs) in seawater samples. DCF-EME method is based on the rapid and simple phase separation of low density organic solvent from the aqueous phase via introducing of a saturated NaHCO3 solution (9.6% w/v) into the acidified sample solution (0.1M of HCl) containing analytes. Thanks to the in situ generation of carbon dioxide (CO2) bobbles intensified by ultrasound radiation, the dispersed extraction solvent was collected to the surface of the aqueous sample and then was narrowed to the capillary part of a special home-made extraction cell for facile retrieving. Under the optimal conditions, the limits of detection were at the range of 2.6–9.2ngL−1 and preconcentration factors were varied between 271 and 307 for different OCPs. The applicability of the developed method was evaluated by the extraction and determination of the target analytes from Caspian seawater samples.
Full text
Available for:
GEOZS, IJS, IMTLJ, KILJ, KISLJ, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UL, UM, UPCLJ, UPUK
In the present study, antifouling paint booster biocides, Irgarol 1051 and diuron were measured in ports and marinas of Bushehr, Iran. Results showed that in seawater samples taken from ports and ...marinas, Irgarol was found at the range of less than LOD to 63.4ngL−1 and diuron was found to be at the range of less than LOD to 29.1ngL−1 (in Jalali marina). 3,4-dichloroaniline (3,4-DCA), as a degradation product of diuron, was also analyzed and its maximum concentration was 390ngL−1. Results for analysis of Irgarol 1051 in sediments showed a maximum concentration of 35.4ngg−1 dry weight in Bandargah marina. A comparison between the results of this study and those of other published works showed that Irgarol and diuron pollutions in ports and marinas of Bushehr located in the Persian Gulf were less than the average of reports from other parts of the world.
•Irgarol and diuron were measured in ports and marinas of Bushehr, Iran.•Irgarol and diuron were detected in 31 and 25% of water samples, respectively.•Higher presence of biocides in dhows mooring spaces was observed.•The area's sediments and water are characterized by low levels of antifoulants.
Full text
Available for:
GEOZS, IJS, IMTLJ, KILJ, KISLJ, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UL, UM, UPCLJ, UPUK, ZRSKP
•Microfunnel-supported LPME for extraction of antifouling agents in seawater samples was developed.•A glass microfunnel device for LPME was designed for solvents less dense than water.•The special ...design of MF makes it convenient to be utilized for a wide range of extraction solvent volume.•The device is tangent to the sample surface reducing the interference in mixing efficiency.•Analysis of samples collected from harbors of Bushehr (IR Iran) was done.
In the present work, microfunnel-supported liquid-phase microextraction method (MF-LPME) based on applying low density organic solvent was developed for the determination of antifoulings (Irgarol 1051, diuron and 3,4-dichloroaniline) from seawater samples. In this method, home-designed MF device was used for facile loading and retrieving of organic solvent during the extraction procedure. The extraction was carried out with introduction of 400μL of toluene via syringe into the MF device placed on the surface of sample solution (300mL) containing analytes. After the extraction, extractant layer was narrowed into the capillary part of MF by pushing the device inside the sample and withdrawn by using a syringe to evaporate by nitrogen purging. The residual redissolved into 50μL methanol, diluted to 100μL with deionized water and injected into the high performance liquid chromatography with UV detection (HPLC–UV). Several factors influencing the extraction such as the type and volume of extraction solvent, sample pH, extraction time and ionic strength were investigated and optimized. Under the optimized conditions, the limits of detection in seawater were 1.4, 4.8 and 1.0ngL−1 for 3,4-dichloroaniline (DCA), diuron and Irgarol 1051, respectively. Enrichment factors were obtained 333, 150 and 373 for DCA, diuron and Irgarol 1051, respectively. The precision of the technique was evaluated in terms of repeatability which was less than 12.0% (n=5). The applicability of the proposed method was evaluated by the extraction and determination of antifoulings from seawater samples collected from harbors of Bushehr located in northern Persian Gulf coast.
Full text
Available for:
GEOZS, IJS, IMTLJ, KILJ, KISLJ, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UL, UM, UPCLJ, UPUK
The applicability of hollow fiber liquid phase microextraction (HF-LPME) for extraction and preconcentration of trace amounts of pioglitazone (PGL) as an anti-diabetic drug in biological fluids, ...prior to determination by high-performance liquid chromatography (HPLC), was evaluated. In this technique, the target drug was extracted into di-
n-hexyl ether immobilized in the wall pores of a porous hollow fiber from 10
mL of the aqueous sample (source phase, SP) with pH 8.0, and then back extracted into the receiving phase (RP) with pH 2.2 located in the lumen of the hollow fiber. The extraction occurred due to a pH gradient between the two sides of the hollow fiber. After extracting for a prescribed time, 24
μL of the RP solution was taken back into the syringe and injected directly into a HPLC instrument for quantification. The Taguchi orthogonal array (OAD) experimental design with an OA
16 (4
5) matrix was employed to optimize the HF-LPME conditions. Different factors affecting the HF-LPME efficiency such as the nature of organic solvent used to impregnate the membrane, pH of the SP and RP, stirring speed, extraction time and ionic strength were studied and optimized. Under the optimum conditions (di-
n-hexyl ether as membrane impregnation solvent, pHs of the SP and RP equal to 8.0 and 2.2, respectively, extraction time of 30
min, stirring speed of 500
rpm and 10% (w/v) NaCl for adjusting the ionic strength), preconcentration factor of 180, linear dynamic range (LDR) of 2.5–250
μg
L
−1 with good correlation of determination (
r
2
>
0.998) and limit of detection (LOD) of 1.0
μg
L
−1 were obtained for the target drug. The percent relative intra-day and inter-day standard deviations (RSDs%) based on five replicate determinations were 4.7 and 15%, respectively. Once LPME was optimized, the performance of the proposed technique was evaluated for the determination of PGL in different types of biological fluids such as plasma and urine samples. The results showed that the proposed HF-LPME method could be successfully applied to determine trace amounts of PGL in biological samples.
Full text
Available for:
GEOZS, IJS, IMTLJ, KILJ, KISLJ, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UL, UM, UPCLJ, UPUK
In this study, liquid-phase microextraction using low-density extraction solvents with microfunnel was applied for the extraction and preconcentration of Bisphenol A and 4-Nonylphenol in aqueous ...samples. The goal of the present method is to develop a special device that allows organic solvent remain on the surface of aqueous phase as a thin layer during the extraction time. At the end of extraction period, organic phase containing the extracted analytes was collected easily and analyzed by HPLC–FLD. Toluene used as extraction solvent and some of experimental parameters were optimized by L
16
Taguchi experimental design. According to the results, the volume of extraction solvent as well as ionic strength showed significant effect on the extraction recovery. Under the optimum conditions (sample volume: 320 mL; pH 8.0; ionic strength: 10% (w/v) NaCl, extraction time: 90 min and extractant: 600 μL toluene), limit of detection, limit of quantification and dynamic linear range of the proposed method for Bisphenol A were calculated as 0.05, 0.2 and 0.2–62.5 μg L
−1
, and for Nonylphenol were obtained as 3.1, 6.2 and 6.2–125 μg L
−1
, respectively.
Full text
Available for:
EMUNI, FIS, FZAB, GEOZS, GIS, IJS, IMTLJ, KILJ, KISLJ, MFDPS, NLZOH, NUK, OILJ, PNG, SAZU, SBCE, SBJE, SBMB, SBNM, UKNU, UL, UM, UPUK, VKSCE, ZAGLJ
Electromembrane extraction coupled with high‐performance liquid chromatography (HPLC) and ultraviolet (UV) detection was developed for the determination of levamisole in some human biological fluids. ...Levamisole migrated from 4 mL of different acidized biological matrices, through a thin layer of 2‐nitrophenyl octyl ether containing 5% tris‐(2‐ethylhexyl) phosphate immobilized in the pores of a porous hollow fiber, into a 20‐μL acidic aqueous acceptor solution present inside the lumen of the fiber. The parameters influencing electromigration were investigated and optimized. Within 15 min of operation at 200 V, levamisole was extracted from different biological fluid samples with recoveries in the range of 59–65%, which corresponded to preconcentration factors in the range of 118–130. The calibration curves showed linearity in the range of 0.5–10, 0.2–10 and 0.1–10 μg/mL for plasma, urine and saliva, respectively. Limits of detection of 0.1, 0.07 and 0.05 μg/mL and limits of quantification of 0.5, 0.2 and 0.1 μg/mL were obtained for plasma, urine and saliva, respectively. The relative standard deviations of the analysis were found to be in the range of 5.6–9.7% (n=3). Electromembrane extraction was successfully processed for determination of levamisole in plasma, urine and saliva samples.
Full text
Available for:
BFBNIB, FZAB, GIS, IJS, KILJ, NLZOH, NUK, OILJ, SAZU, SBCE, SBMB, UL, UM, UPUK
In the present work, a simple and high sensitive method based on hollow fiber liquid phase microextraction (HF-LPME) was developed followed by high performance liquid chromatography (HPLC) for ...determination of ultra-trace amounts of Se(IV) after derivatization in biological and natural water samples. Se(IV) was complexed with
o-phenylenediamine to form piazselenol. The formed piazselenol was extracted into 20
μL of 1-octanol located in the lumen of a hollow fiber and the solution was injected into HPLC-UV for analysis. Using the Taguchi method, an orthogonal array design (OAD), OA
16 (4
5) was employed to optimize the HF-LPME of piazselenol. The effect of five experimental factors (each factor at four levels) including the volume of the organic phase, extraction time, pH of the solution, stirring rate and ionic strength on the extraction efficiency of piazselenol was studied and optimized. The maximum extraction efficiency of piazselenol was obtained at 20
μL of 1-octanol as the extracting solvent, 30
min extraction time, pH 2, stirring rate of 500
rpm and 30% (w/v) NaCl. Under the optimum conditions, preconcentration factors up to 130 were achieved and the relative standard deviation (%RSD) of the method was <3.7% for different concentrations of Se(IV). The calibration curves were obtained in the ranges of 0.2–100 and 0.05–10
μg
L
−1 for the 11 and 50
mL of the sample volumes with reasonable linearity, respectively (
r
2
>
0.995). The limits of detection (LOD) were 0.1 and 0.02
μg
L
−1 for the 11 and 50
mL sample volumes, respectively (
S/
N
=
3). Finally, the applicability of the proposed method was evaluated by the extraction and determination of Se(IV) in the plasma, urine and water samples.
Full text
Available for:
GEOZS, IJS, IMTLJ, KILJ, KISLJ, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UL, UM, UPCLJ, UPUK
