Determination and Stability of Phenmediphan, Ethofumesate and Fenamiphos in Ground Water Samples Using Automated Solid Phase Extraction Cartridges Followed by Liquid Chromatography High Flow Pneumatically Assisted Electrospray Mass Spectrometry

Abstract

The determination and stability of polar pesticides phenmediphan, ethofumesate and fenamiphos in ground water samples was subjected to analysis with solid phase extraction (SPE) followed by liquid chromatographyhigh flow pneumatically assisted electrospray mass spectrometry (LC-ESP-MS). Pesticides were spiked at 6 μg/L in ground water samples and 80 mL were preconcentrated by using an Automated Sample Preparation with Extraction Columns (ASPEC XL) system.

After preconcentration, several different storage conditions were tested, which included storage at 4[ddot]C, at −20[ddot]C and at room temperature using styrene divinylbenzene (SDB) cartridges. The percentage of degradation varied from 20 to 80% for all the studied pesticides after 20 days of storage at room temperature. Phenmediphan and ethofumesate were stable at 4[ddot]C and −20[ddot]C during all the studied period whereas fenamiphos was recovered only 32 and 50% at 4 [ddot]C and −20[ddot]C, respectively, after 80 days of storage.

The L.O.D under LC-ESP-MS and SIM conditions were between 10–20 pg, 5–60 times lower as compared to LC-thermospray-MS with no thermal degradation of phenmediphan. This higher sensitivity of LC-ESP-MS permitted the determination of fenamiphos sulphoxide formed during the extraction and storage and the identification of the interferences present in the cartridges e. g., diethyl and di-n-butyl phthalates.

Key Words:

• Polar pesticides
• solid phase extraction
• stability studies
• ground water
• electrospray mass spectrometry