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A validated matrix solid-phase dispersion method for the extraction of organophosphorus pesticides from bovine samples
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文摘
A method based on matrix solid-phase dispersion (MSPD) was developed for the quantitative extraction of five organophosphorus (OPPs) pesticides from bovine samples. The determination was carried out by high performance liquid chromatography (HPLC) with diode array spectrophotometric UV detection. The MSPD extraction with octadecylsilyl (C18) sorbent combined with a silica gel clean-up and acetonitrile elution was optimised for chlorpyrifos, chlorfenvinphos, diazinon, fenitrothion, and parathion-methyl. The method was validated, yielding recovery values higher than 94 % , except for chlorfenvinphos in liver (55 % ), and precision values, expressed as relative standard deviations (RSDs), which were less than or equal to 15 % in liver and 11.5 % in muscle at spiking levels of 0.25, 2.5 and 5 μg g−1. Linearity was studied from 0.5 to 15 μg g−1, and the limits of detection (LODs) were found to be lower than 0.1 μg g−1. This method was applied to the analysis of real samples with confirmative analyses performed using gas chromatography–mass spectrometry (GC–MS) in selected ion monitoring mode (SIM).

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