Toprak Örneklerindeki Propaklor ve Prometrin Herbisitlerinin Sıvı Kromatografisi Analizleri Öncesinde Supramoleküler Çözücü Esaslı Mikroekstraksiyonu

Supramoleküler çözücüler (SUPRASs), amfifillerin kendiliğinden bir birleşme prosesi ile meydana getirdiği nano yapılı sıvılardır ve örnek hazırlama basamağında daha çevre dostu olmaları nedeniyle moleküler organik çözücülere bir alternatif oluştururlar. Bu çalışmada, toprak örneklerindeki propaklor ve prometrin herbisitlerinin mikroekstraksiyonu için SUPRAS esaslı bir analitik metot önerilmektedir. Önerilen metot, 300 mg toprak numunesinin 300 μL SUPRAS ile 8 dakika boyunca vorteks ile karıştırılmasını, ardından faz ayrımı için santrifüjlemeyi ve ultraviyole dedektörlü sıvı kromatografisiyle SUPRAS fazının doğrudan analizini içermektedir. Optimize edilen ekstraksiyon koşullarında, herbisitler için ekstraksiyon verimleri % 81 ile % 87 arasında değişim göstermiştir. Metot algılama limitleri, propaklor ve prometrin için sırasıyla 0.07 μg/g ve 0.01 μg/g olarak bulunmuştur. Herbisitler için bulunan bağıl standart sapma değerleri gün-içi ve günler-arası tekrarlanabilirlik olarak sırasıyla % 8.8 ve % 12.1’den daha düşük bulunmuştur. İlgili herbisitlerin Zonguldak bölgesinden toplanan toprak örneklerinden mikroekstraksiyonu verimli bir şekilde yapılmıştır. Standart madde ilavesi yapılan toprak örnekleri için elde edilen geri kazanım değerleri %80 ile %108 arasında değişim göstermiştir.

Supramolecular Solvent-Based Microextraction of Propachlor and Prometryn Herbicides in Soil Samples Prior to Liquid Chromatographic Analysis

Supramolecular solvents (SUPRASs) are the nano-structured liquids generated from amphiphiles through a self-assembly process, and constitute an alternative to molecular organic solvents with becoming more environmentally friendly in sample preparation step. In this study, a SUPRAS-based analytical method has been proposed for the microextraction of propachlor and prometryn herbicides in soil samples. The method involved the vortex mixing of the 300 mg of soil sample with 300 μL of SUPRAS for 8 min, subsequent centrifugation for the phase separation, and direct analysis of the SUPRAS phase by liquid chromatography with ultraviolet detection. Under optimal extraction conditions, the extraction recoveries for the herbicides ranged from 81 to 87 %. The method detection limits for propachlor and prometryn were 0.07 and 0.01 μg/g, respectively. Relative standard deviations obtained for the herbicides were less than 8.8 % and 12.1 % for intra-day and inter-day precisions, respectively. The microextraction of related herbicides from soil samples collected from the Zonguldak region was carried out efficiently. The recoveries obtained from spiked soil samples ranged from 80 to 108 %.

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