Determination of phthalate esters in seawater of Chabahar Bay using dispersive liquid-liquid microextraction coupled with GC-FID

2017 ◽  
Vol 77 (7) ◽  
pp. 1782-1790 ◽  
Author(s):  
Beheshteh Ajdari ◽  
Mahmoud Nassiri ◽  
Mir Mahdi Zahedi ◽  
Morteza Ziyaadini

Abstract Phthalate esters (PEs), a group of environmental pollutants which are possibly carcinogenic to humans, have been detected in seawater. Seven PEs in seawater were quantitatively determined by using gas-chromatography flame ionizing detection after executing dispersive liquid-liquid microextraction. The suggested method is optimized for microextraction and determination of PEs in artificial sea water. Factors affecting the microextraction procedure such as the type and volume of extracting and dispersive solvents (carbon tetrachloride, 20 μL; methanol, 0.5 mL), extraction time and pH (7) were investigated. Under optimum conditions, the limit of detection of the analytes were obtained between 0.04 and 4.52 μg·L−1, and linearity and linear range were of 0.999 ≥ R2 ≥ 0.994 and 10–560 μg·L−1 respectively. Enrichment factors were found in the range of 761–827 fold, while the relative standard deviations of the analytes were between 0.17 and 7.5% (n = 6) for real sea water samples. Using this method, total PEs content of seawater from several locations in Chabahar Bay (the southeast part of Iran) was estimated 2.33–90.45 μg·L−1.

2014 ◽  
Vol 2014 ◽  
pp. 1-4 ◽  
Author(s):  
J. Pérez-Outeiral ◽  
E. Millán ◽  
R. Garcia-Arrona

A simple and inexpensive method for cadmium determination in water using dispersive liquid-liquid microextraction and ultraviolet-visible spectrophotometry was developed. In order to obtain the best experimental conditions, experimental design was applied. Calibration was made in the range of 10–100 μg/L, obtaining good linearity (R2 = 0.9947). The obtained limit of detection based on calibration curve was 8.5 μg/L. Intra- and interday repeatability were checked at two levels, obtaining relative standard deviation values from 9.0 to 13.3%. The enrichment factor had a value of 73. Metal interferences were also checked and tolerable limits were evaluated. Finally, the method was applied to cadmium determination in real spiked water samples. Therefore, the method showed potential applicability for cadmium determination in highly contaminated liquid samples.


Author(s):  
Mohamed A Hammad ◽  
Amira H Kamal ◽  
Reham E Kannouma ◽  
Fotouh R Mansour

Abstract A validated method for preconcentration and determination of nateglinide in plasma was developed using vortex-assisted dispersive liquid–liquid microextraction. Different variables that affect extraction efficiency were studied and optimized, including type and volume of extractant, type and volume of disperser, pH of diluent, salt addition effect, centrifugation and vortex time. Nateglinide was extracted using 30 μL of 1-octanol as an extractant and 200 μL of methanol as a disperser. The enrichment factor reached 330 under the optimum conditions. High-performance liquid chromatography/ultraviolet was used for detection using phosphate buffer (pH 2.5, 10 mM): acetonitrile (45:55, v/v) as a mobile phase at a flow rate of 1 mL/min. The method was linear over the range of 50–20,000 ng/mL with a limit of detection of 15 ng/mL (signal-to-noise ratio = 3). Intra- and inter-day precision had %relative standard deviation <6% (n = 3) and the %recoveries were found to be between 102.5 and 105.9%. The proposed method is simple, sensitive, eco-friendly, cost-effective and powerful for microextraction of nateglinide from human plasma samples.


Water ◽  
2019 ◽  
Vol 11 (8) ◽  
pp. 1581 ◽  
Author(s):  
Hryniewicka ◽  
Starczewska ◽  
Gołębiewska

Dispersive liquid–liquid microextraction based on solidification of floating organic droplet (DLLME-SFO) was applied to isolate budesonide (BUD) and sulfasalazine (SULF) from aqueous samples. The effects of different parameters on the efficiency on the extraction such as type of extrahent and dispersive solvent, ionic strength, pH of sample, and centrifugation time were investigated. Moreover, the influence of foreign substances on a studied process was tested. The calibration curves were recorded. The linearity ranges for BUD and SULF were 0.022–8.611 µg mL−1 and 0.020–7.968 µg mL−1 with the limit of detection (LOD) 0.011 µg mL−1 and 0.012 µg mL−1, respectively. The enrichment factors (EF) for two analytes were high: for BUD it was 145.7 and for SULF, 119.5. The elaborated procedure was applied for HPLC-UV determination of these analytes in water and wastewater samples.


2012 ◽  
Vol 190-191 ◽  
pp. 603-608 ◽  
Author(s):  
Chen Zhang ◽  
Long Jiang ◽  
Chong Meng ◽  
Xiao Peng Li ◽  
Yu Li

An ultrasound-assisted dispersive liquid-liquid micro-extraction method based on solidification of floating organic drop (UAE/DLLME/SFO) was established for the determination of PAHs in soils. Dichloromethane was used as solvent for the analytes in the soil by ultrasonic assistant extraction (UAE), the solvent was purified and concentrated by silica gel column chromatography and nitrogen flowing concentrator, respectively. The recoveries of the method were in the range 46.22-101.86%, and the relative standard deviations (RSD) were 3.03-7.80%. The linear range was 0.02-0.4mg/kg(0.02-0.5mg/kg), and the limit of detection (LOD) was 0.17-29.13µg/kg. The method was applied to the real soil samples around wells of an oilfield; the relative recoveries of the ANY, ANA, FLU, PHE, ANT, FLT, PYR, BaA were 47.12-116.96%, while the recoveries of NAP, CHR, BbF, BkF, BaP, DBA, BPE, IPY were 17.75-63.29%.


2021 ◽  
Vol 4 (1) ◽  
Author(s):  
Siroos Shojaei ◽  
Saeed Shojaei ◽  
Arezoo Nouri ◽  
Leila Baharinikoo

AbstractAs the world population continues to grow, so does the pollution of water resources. It is, therefore, important to identify ways of reducing pollution as part of our effort to significantly increase the supply of clean and safer water. In this study, the efficiency of ultrasound-assisted dispersive liquid–liquid microextraction (UA-DLLME) as a fast, economical, and simple method for extraction malachite green (MG) and rhodamine B (RB) dyes from water samples is investigated. In optimal conditions, the linear dynamic range (LDR) for RB and MG is 7.5–1500 ng mL−1 and 12–1000 ng mL−1, respectively. The limit of detection (LOD) is 1.45 ng mL−1 and 2.73 ng mL−1, and limit of quantification (LOQ) is 4.83 ng mL−1 and 9.10 ng mL−1 for RB and MG, respectively. Extraction efficiency is obtained in the range of 95.53–99.60%. The relative standard deviations (RSD) in real water and wastewater samples are less than 3.5. The developed method is used successfully in the determination of RB and MG dyes from water samples and there are satisfactory results.


2020 ◽  
Vol 32 (12) ◽  
pp. 3191-3196
Author(s):  
Intizam Ahmadov

In this study, a new method was developed for the spectrophotometric determination of zirconium by the procedure of dispersive liquid-liquid microextraction based on the solidification of floating organic droplets (DLLME-SFO). o-Nitrobenzene-azopyrocatechol (o-NBAP) and non-ionic surfactant (OP-10) were used in the complex formation. At the first stage, a separation and solidification processes were carried out, after which the solidified samples were examined by spectrophotometric method. The effect of various parameters viz. pH effect, ion resistance, ligand effect, volume and type of extraction and dispersion solution, extraction time and temperature effect were studied. The results of the experiment were optimized with design programs. The calibration curve was linear ranging from 0.5 to70 μg L-1, with a correlation coefficient of 0.998. The limit of detection (LOD) is 0.12 μg L-1, the limit of quantification (LOQ) is 0.40 μg L-1 and the relative standard deviation (RSD) at 60 μg L-1 is 1.6% (n=6). This method was also applied to determine zirconium in various water samples. The obtained reextraction amount was 98-110%.


2014 ◽  
Vol 97 (1) ◽  
pp. 183-187 ◽  
Author(s):  
Run-Zhen Fan ◽  
Congyun Liu ◽  
Wenqing Jiang ◽  
Xiaonan Wang ◽  
Fengmao Liu

Abstract Ultrasound-assisted dispersive liquid–liquid microextraction (UA-DLLME) based on solidification of the floating organic solvent droplets (SFO) combined with HPLC was used for determination of five fungicides in fruit juice samples. 1-Dodecanol, which has a low density and low toxicity, was used as the extraction solvent in UA-DLLME. The solidification of floating organic dropletsfacilitates the transfer of analytes from the aqueous phase to the organic phase. This method was easy, quick, inexpensive, precise, and linear over a wide range. Under the optimized conditions, the enrichment factors for a 5 mL fruit juice sample were 25 to 56, and the LODs for the five fungicides ranged from 5 to 50 μg/L. The average recoveries ranged from 71.8 to 118.2% with RSDsof 0.9 to 13.9%. Application of the DLLME-SFO technique allows successful separation and preconcentration of the fungicides at a low concentration level in fruit juice samples.


2020 ◽  
Vol 3 (1) ◽  
pp. 23 ◽  
Author(s):  
Ivan Notardonato ◽  
Sergio Passarella ◽  
Giuseppe Ianiri ◽  
Cristina Di Fiore ◽  
Mario Vincenzo Russo ◽  
...  

In this paper, an analytical protocol was developed for the simultaneous determination of phthalates (di-methyl phthalate DMP, di-ethyl phthalate DEP, di-isobutyl phthalate DiBP, di-n-butyl phthalate DBP, bis-(2-ethylhexyl) phthalate DEHP, di-n-octyl phthalate DNOP) and bisphenol A (BPA). The extraction technique used was the ultrasound vortex assisted dispersive liquid–liquid microextraction (UVA-DLLME). The method involves analyte extraction using 75 µL of benzene and subsequent analysis by gas chromatography combined with ion trap mass spectrometry (GC-IT/MS). The method is sensitive, reliable, and reproducible with a limit of detection (LOD) below 13 ng g−1 and limit of quantification (LOQ) below 22 ng g−1 and the intra- and inter-day errors below 7.2 and 9.3, respectively. The method developed and validated was applied to six honey samples (i.e., four single-use commercial ones and two home-made ones. Some phthalates were found in the samples at concentrations below the specific migration limits (SMLs). Furthermore, the commercial samples were subjected to two different thermal stresses (24 h and 48 h at 40 °C) for evidence of the release of plastic from the containers. An increase in the phthalate concentrations was observed, especially during the first phase of the shock, but the levels were still within the limits of the regulations.


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