Simultaneous Determination of Selected Insecticides and Atrazine in Soil by MAE-GC-ECD

• Autorzy: Barchańska H. , Czalicka M. , Giemza A.

Warianty tytułu

PL

Równoczesne oznaczanie wybranych insektycydów i atrazyny w glebie techniką MAE-GC-ECD

• Języki publikacji: EN

Abstrakty

EN

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 ěg/mL – 18 ěg/mL and 2 ěg/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.

PL

Opracowano procedurę MAE–GC–ECD umożliwiającą równoczesną ekstrakcję i oznaczanie insektycydów: aldryny, dieldryny i endryny oraz herbicydu: atrazyny z gleb. Zastosowana metoda GC–ECD charakteryzuje się granicą wykrywalności w zakresie 12–18 žg/ml dla insektycydów oraz 2 žg/m for dla atrazyny. W celu opracowania procedury analitycznej o wysokim odzysku analitów i granicy oznaczalności typowej dla analizy śladowej (100 ppm lub 100 mg/g wg. IUPAC) przeprowadzono badania z zastosowaniem ekstrakcji rozpuszczalnikowej wspomaganej ultradźwiękami (UAE) oraz mikrofalami (MAE) dla różnych rozpuszczalników. Dokonano porównania precyzji oraz odzysków analitów dla obu technik ekstrakcyjnych. Wydzielanie insektycydów z próbek gleb na drodze ekstrakcji rozpuszczalnikowej wspomaganej ultradźwiękami przeprowadzono z odzyskiem 40–85% (CV: 1,3–5,0%), natomiast atrazyny 15% (CV: 8–18%). Najwyższą precyzją i odzyskiem charakteryzowała się metoda MAE z zastosowaniem mieszaniny n-heksan–aceton. Odzyski mieściły się w tym przypadku w zakresie 70–85% (CV: 0,4–2,2%) dla insektycydów oraz 84% (CV: 5,3%) dla atrazyny. Opisana procedura MAE–GC–ECD umożliwia ekstrakcję i oznaczenie aldryny, dieldryny, endryny oraz atrazyny w próbkach gleb. Charakteryzuje się wysokimi odzyskami, precyzją i granicami wykrywalności mieszczącymi się w granicach 6–8 ng/g, w przypadku insektycydów oraz 1,5 ng/g dla atrazyny. Metodyka MAE–GC–ECD została zastosowana do oznaczanie wymienionych pestycydów w próbkach gleb pobranych z terenów rolniczych oraz przemysłowych. We wszystkich próbkach gleb oznaczono atrazynę, której stężenie mieściło się w granicach od 0,0187 mg/g do 0,1107 mg/g w zależności od pochodzenie próbki. Aldryna i dieldryna została wykryta w dwóch próbkach na poziomie poniżej granicy oznaczalności.

Słowa kluczowe

EN

soil; pesticides; MAE; UAE; GC-ECD

PL

gleba; procedura MAE-GC-ECD; równoczesna ekstrakcja; oznaczanie insektycydów

• Wydawca: Institute of Environmental Engineering, Polish Academy of Sciences
• Czasopismo: Archives of Environmental Protection
• Rocznik: 2013
• Tom: Vol. 39, no. 1
• Strony: 27--40
• Opis fizyczny: Bibliogr. 53 poz., tab., wykr.

Twórcy

autor

Barchańska H.

autor

Czalicka M.

autor

Giemza A.

• Department of Analytical Chemistry, Silesian University of Technology, Gliwice, M. Strzody 7, Poland,

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