Determination of endosulfan isomers and their metabolites in tap water and commercial samples using microextraction by packed sorbent and GC–MS

Abstract

A simple, rapid, accurate and sensitive method using microextraction by packed sorbent (MEPS) followed by GC-MS has been pursued for the determination of organochlorine insecticide endosulfan isomers (α and β) and their metabolites (ether, lactone and sulfate). MEPS is a miniaturised version of SPE employing C18 packing material. It is very efficient technique as it employs as low as 10 μL of sample volume. The distinct feature of MEPS is the magnitude of the elution volume that could be directly injected to GC system. Various parameters such as extraction cycles, washing solvent, elution solvent, elution volume and pH, which influenced the MEPS performance, were tested and optimised. The calibration curves were obtained in the concentration range 1-500 ng/mL. The results showed a close correlation coefficient (R(2) > 0.991) for all analytes in the calibration range studied. The LOD and LOQ obtained for GC-MS under selected ion monitoring acquisition are between 0.0038-0.01 and 0.0125-0.033 ng/mL, respectively. The developed method is applicable for the quantification of these compounds in tap water and commercial samples. This method has been shown to be selective as no interferences from endogenous substances were detected by analysis. This method not only decreases sample preparation time but is cheaper, eco-friendly and easier to perform compared to traditional techniques.

Current trends on microextraction by packed sorbent – fundamentals, application fields, innovative improvements and future applications

“…The use of pesticides in modern agriculture is an indispensable measure to protect crops from diseases and pests, therefore ensuring their economic viability. 75,76 Pesticide usage, however, is not limited to industrial applications, being nowadays also widespread in homegrown applications. For this reason, there are more than 1100 active compounds registered and available in the European Union (EU) markets!…”

“…Taghani et al, for instance, proposed nanodiatomite 77 and carboxyl-purified multiwalled carbon nanotubes (CNTs) 84 as sorbents for the preconcentration of several OCPs (Table 2). In turn, Kaur et al 75 used the C 18 MEPS sorbent to extract endosulfan and its metabolites in tap water.…”

Determination of Concentration for Some Priority Substances in Paddy Fields of Ergene River, Meriç River, and Yenikarpuzlu Dam, Turkey

“…Acute toxicity is a colorless, solid agricultural chemical prohibited due to its bioaccumulative potential and endocrine disrupting effects [4][5][6]. EN residues in nature are also known to remain in the soil for at least 6 years [7,8]. Therefore, it requires examination of the soil contaminated with EN, the product grown in soil, sediment and the water used.…”

“…The extensively used high sensitivity analytical techniques for the determination of EN and PAHs at low concentrations in environmental samples are GC-MS [6,8,20,21], HPLC-MS [10,22]. The separation and preconcentration techniques for pesticides are solid phase extraction (SPE) [21,23,24], solid phase micro extraction (SPME) [21,22,25] and sonication [22,26], which are used to solve these problems in analysis of EN and PAHs.…”

Self-made microextraction by packed sorbent device for the cleanup of polychlorinated biphenyls from bovine serum

“…Additionally, one MEPS device can be reused more than 100 times, even for particularly complex samples. This technique has been successfully used to extract a wide range of analyses in different matrices, such as water, groundwater, wine, urine, plasma, saliva, etc .…”