scholarly journals Simultaneous Determination of Selected Insecticides and Atrazine in Soil by Mae–GC–ECD

2013 ◽  
Vol 39 (1) ◽  
pp. 27-40 ◽  
Author(s):  
Hanna Barchańska ◽  
Marianna Czalicka ◽  
Anna Giemza

Abstract The procedure for simultaneous extraction from soil and determination by means of GC-ECD insecticides: aldrin, dieldrin, endrin and herbicide: atrazine was worked out. The proposed GC-ECD technique provides limits of detection in range 12 μg/mL - 18 μg/mL and 2 μg/mL, for insecticides and atrazine, respectively. Two different types of extraction: microwave assisted extraction (MAE) and ultrasound assisted extraction (UAE) with different solvents were tested to choose the procedure that provides the highest recoveries of analytes and low detection limits, typical for trace analysis (100 ppm or 100 mg/g, IUPAC). On the basis of recoveries and precision both extraction methods were compared. The insecticides recovery from soil samples obtained by UAE were in range 40-85%, coefficient of variation (CV): 1.3-5.0%, whereas for atrazine recovery was below 15% (CV: 8-18%). The most efficient and precise extraction procedure turned out to be MAE with n-hexane: acetone. The recoveries were in range 70-85% for insecticides and 84% for atrazine, CV: 0.4-2.2% and 5.3% for insecticides and atrazine, respectively. The presented MAE-GC-ECD procedure enables extraction and determination of aldrin, dieldrin, endrin and atrazine in soil samples with high recoveries, precision and limits of detections in range 6 ng/g - 8 ng/g in the case of insecticides and 1.5 ng/g for atrazine. The MAE-GC-ECD procedure was applied for the above mentioned pesticides determination in environmental samples. Soils were collected in agricultural as well as rural areas in Poland. In all cases atrazine was determined in concentration range: 0.0187 mg/g - 0.1107 mg/g. Aldrin and dieldrin was detected in soil samples from two locations.

Minerals ◽  
2021 ◽  
Vol 11 (10) ◽  
pp. 1103
Author(s):  
Mceliseni Zuma ◽  
Philiswa Nomngongo ◽  
Nomvano Mketo

The world during the COVID-19 pandemic has led to extensive use of virtual activities by means of electronic devices, which are made up of rare earth elements (REEs). This means that quantitative knowledge of REEs in various resources is crucial for the development of effective recovery methods. Therefore, this report describes a simple microwave assisted ashing followed by ultrasound-assisted extraction (MAA-UAE) for quantitative determination of REEs in coal samples using inductively coupled plasma-optical emission spectroscopy (ICP-OES). Firstly, coal samples were ashed at 55 °C for 4.5 h to form white ashes, which were then treated with dilute HNO3 acid under ultrasonication to enhance the extraction of REEs. The quantitative recoveries (86–120%) of REEs were obtained when 1 mol L−1, 0.1 g, 40 °C, 20 min, and high frequency were applied for [HNO3], sample mass, ultrasonic bath temperature, extraction time, and ultrasonic bath frequency, respectively. The method detection limits of the proposed MAA-UAE method were between 0.0075 and 0.59 µg g−1 with satisfactory precision (<5%). The concentration levels of REEs in South African coals ranged from 1.4 to 105 µg g−1, suggesting that this coal can be a resource for REEs.


Molecules ◽  
2021 ◽  
Vol 26 (10) ◽  
pp. 2879
Author(s):  
Aleksandar Radivojac ◽  
Oskar Bera ◽  
Zoran Zeković ◽  
Nemanja Teslić ◽  
Živan Mrkonjić ◽  
...  

Consumers are becoming more mindful of their well-being. Increasing awareness of the many beneficial properties of peppermint essential oil (EO) has significantly increased product sales in recent years. Hydrodistillation (HD), a proven conventional method, and a possible alternative in the form of microwave-assisted hydrodistillation (MWHD) have been used to isolate peppermint EO. Standard Soxhlet and alternatively supercritical fluid (SFE), microwave-assisted, and ultrasound-assisted extraction separated the lipid extracts. The distillations employed various power settings, and the EO yield varied from 0.15 to 0.80%. The estimated environmental impact in terms of electricity consumption and CO2 emissions suggested that MWHD is an energy efficient way to reduce CO2 emissions. Different extraction methods and solvent properties affected the lipid extract yield, which ranged from 2.55 to 5.36%. According to the corresponding values of statistical parameters, empiric mathematical models were successfully applied to model the kinetics of MWHD and SFE processes.


2016 ◽  
Vol 51 (4) ◽  
pp. 344-356 ◽  
Author(s):  
Hing-Biu Lee ◽  
M. Lewina Svoboda ◽  
Thomas E. Peart ◽  
Shirley Anne Smyth

A microwave-assisted extraction method for the determination of 15 alkyl, aryl, and halogenated phenols in sewage sludge and biosolids samples was developed and optimized. The effects of solvent, temperature, time, moisture content, acid, and number of extractions on the recovery of phenols were evaluated. Results indicated that extraction solvent had the greatest impact on the recovery of all phenols while pH had the largest effect on recovery of hexachlorophene and pentachlorophenol. Wet sludge samples were extracted with acetone-hexane mixture in the presence of glacial acetic acid. The extract was evaporated, acetylated by acetic anhydride and cleaned up by silica gel. For dry sludge samples, an optional procedure for the simultaneous extraction and acetylation of phenols was also proposed. Triclosan (TCS) and the alkyl and aryl phenols in sludge extracts were analyzed by gas chromatography-mass spectrometry (GC-MS) in electron-impact mode while polyhalogenated phenols were analyzed by GC-MS in negative ion chemical ionization mode. Method detection limits were ca. 200 ng/g for nonylphenol, &lt;25 ng/g for TCS and other alkyl and aryl phenols, and &lt;5 ng/g for other halogenated phenols. This method has been applied to the determination of phenolic compounds in over 150 sludge and biosolids samples since 2009.


2008 ◽  
Vol 91 (1) ◽  
pp. 174-180 ◽  
Author(s):  
Mercedes Barriada-Pereira ◽  
Iván Iglesias-García ◽  
María J Gonzlez-Castro ◽  
Soledad Muniategui-Lorenzo ◽  
Purificación López-Maha ◽  
...  

Abstract This paper describes a comparative study of 2 extraction methods, pressurized liquid extraction (PLE) and microwave-assisted extraction (MAE), for the determination of organochlorine pesticides (OCPs) in fish muscle samples. In both cases, samples were extracted with hexaneacetone (50 + 50), and the extracts were purified by solid-phase extraction using a carbon cartridge as the adsorbent. Pesticides were eluted with hexaneethyl acetate (80 + 20) and determined by gas chromatography with electron-capture detection. Both methods demonstrated good linearity over the range studied (0.0050.100 g/mL). Detection limits ranged from 0.029 to 0.295 mg/kg for PLE and from 0.003 to 0.054 mg/kg for MAE. For most of the pesticides, analytical recoveries with both methods were between 80 and 120, and the relative standard deviations were &lt;10. The proposed methods were shown to be powerful techniques for the extraction of OCPs from fish muscle samples. Although good recovery rates were obtained with both extraction methods, MAE provided advantages with regard to sample handling, cost, analysis time, and solvent consumption. Acceptable validation parameters were obtained although MAE was shown to be more sensitive than PLE.


2017 ◽  
Vol 12 (3) ◽  
pp. 1934578X1701200 ◽  
Author(s):  
Eleni Kollia ◽  
Panagiota Markaki ◽  
Panagiotis Zoumpoulakis ◽  
Charalampos Proestos

Extracts and infusions of wild artichoke ( Cynara cardunculus L.) and globe artichoke ( C. scolymus L.) (heads, bracts and stems) were examined for their total phenolic content (TPC) and their antioxidant activity after performing Classical Extraction (CE) and Ultrasound-Assisted Extraction (UAE). UAE proved to be more effective, since extracts exhibited higher antioxidant activity and TPC values than CE extracts and infusions. Moreover C. cardunculus heads extract using UAE, displayed the maximum TPC values (1.57 mg gallic acid equivalents (GAE) g−1 fresh weight (fw)), the highest DPPH• scavenging activity (IC50; 0.91mg mL−1) and the highest ABTS•+ radical scavenging capacity (2.08 mg Trolox Equivalents (TE) g−1 fw). Moreover, the effect of different concentrations of C. cardunculus head extracts (showing the highest TPC and antioxidant activity) on Aspergillus parasiticus growth was estimated in AFPA medium. The maximum inhibition was found to be ~42.1% in comparison with the control.


2016 ◽  
Vol 8 (35) ◽  
pp. 6554-6559 ◽  
Author(s):  
Danilo J. Leao ◽  
Mario M. Silva Junior ◽  
Jucelino B. Silva Junior ◽  
Daiane A. F. de Oliveira ◽  
Antonio F. S. Queiroz ◽  
...  

An extraction procedure involving ultrasound assisted radiation was proposed for the determination of mercury in river sediment samples using cold vapour atomic absorption spectrometry (CV AAS).


2006 ◽  
Vol 89 (5) ◽  
pp. 1403-1409 ◽  
Author(s):  
Radoslav Halko ◽  
Carolina PadrÓn Sanz ◽  
Zoraida Sosa Ferrera ◽  
JosÉ Juan Santana RodrÍguez

Abstract A simple and fast analytical method was developed for the determination of benzimidazole fungicides (benomyl, carbendazim, thiabendazole, and fuberidazole) in soil samples. The analytes were extracted from the soil samples by means of conventional microwave-assisted extraction, using the non-ionic surfactants polyoxyethylene 10 lauryl ether (POLE) and oligoethylene glycol monooalkyl ether (Genapol X-080) as extractants. Determinations were made by using liquid chromatography with direct fluorescence detection. The use of an analytical column Symmetry C-18 offered short retention times of analytes without the need of any pH regulators with mobile phase methanolwater (50 + 50, v/v). The best results were obtained using 5% (v/v) POLE as extractant with recoveries of the fungicides in spiked soil samples between 71 and 105%. The results were compared with those obtained when Soxhlet extraction was applied to the same soil samples.


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