Solid-Phase Extraction and Cleanup of Organophosphorus Pesticide Residues in Bovine Muscle with Gas Chromatographic Detection

Abstract

The purpose of this investigation is to develop a rapid and simple method for the assessment of organophosphorus pesticides in bovine muscle by using solid-phase extraction (SPE). After extraction with ethyl acetate (EtOAc) the homogenate is centrifuged and filtered through sodium sulfate. The fat is precipitated in methanol by cooling and the extract is diluted with water and passed through a SPE column (Isolute ENV+). After elution with EtOAc, evaporation, and redissolution, the sample is injected into a gas chromatographic (GC) capillary column DB-1701 and detected by a flame photometric detector. Recoveries from bovine muscle fortified with 12 pesticides between 4 and 65 microg/kg include three levels ranging between 59% and 109% for ten of them. The two most polar pesticides (metamidophos and acephate) are not successful. The relative standard deviations are between 1% and 10% for the ten pesticides. A simplex method is used to optimize the GC conditions.

Organophosphorus pesticides residues in Italian raw milk

“…The main features of the method chosen were the short time of analysis and its effectiveness also with the most polar pesticides (i.e. acephate and methamidophos) (Kuivinen & Bengtsson, 2002). The limits of detection (LOD) and quantification (LOQ) estimated as those concentrations of analyte which yield a signal-to-noise (S/N) ratio respectively of at least 3/1 and 10/1, were 1 mg/kg and 5 mg/kg respectively (Pagliuca et al 2005); therefore, it was possible to detect and quantify OPP residues below the MRL set by European Commission (The European Commission, 2003) ( Table 1).…”

The Diagnostic Approach and Public Health Implications of Phorate Poisoning In a California Dairy Herd

“…There are very few studies that focus on the detection of phorate and its metabolites in edible tissue of animal origin even though there is risk to humans for low level exposure to phorate through the food supply [14][15][16][17][18]. In the reported mortality event on the dairy, a bulk milk tank sample was collected on Day 1 and found to be negative for phorate at a limit of detection of 10 ng/ml.…”

Triclopyr 3, 5, 6-Trichloro-2-Pyridinyl Clean-Up Procedure from Soil, Sediment and Water Samples using SPE-HPLC-VWD

“…Therefore, 3 mL sample was considered the best (Ferenc & Biziuk 2006). behaviour of triclopyr made it difficult to adjust to an appropriate pH for consistent and quantitative extraction (Kuivinen & Bengtsson 2002 …”