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Determination of organophosphorus pesticides by gas chromatography with mass spectrometry using a large‐volume injection technique after magnetic extraction
Authors:Maryam Nedaei  Ali‐Reza Salehpour  Shahla Mozaffari  Seyedeh Mahboobeh Yousefi  Seyed Reza Yousefi
Affiliation:1. Department of chemistry, Payame Noor University, Tehran, Iran;2. Analytical Laboratory, School of Chemical Engineering, College of Engineering, University of Tehran, Tehran, Iran;3. NFCRS, Nuclear Science and Technology Research Institute, Tehran, Iran
Abstract:A fast and efficient method was developed for the extraction and determination of organophosphorus pesticides in water samples. Organophosphorus pesticides were extracted by solid‐phase extraction using magnetic multi‐walled carbon nanotubes and determined by gas chromatography with ion‐trap mass spectrometry. Parameters affecting the extraction were investigated. Under optimum conditions of the method, 10 mg magnetic multi‐walled carbon nanotubes were added into 10 mL sample. After 2 min, adsorbent particles settled at the bottom of test tube with a magnet. After removing aqueous supernatant, the analytes were desorbed with acetonitrile. Then, 70 μL of acetonitrile phase was injected into the gas chromatography and mass spectrometry system that had an ion‐trap analyzer. To achieve high sensitivity, the large‐volume‐injection technique was used with a programmed temperature vaporization inlet, and the ion‐trap mass spectrometer was operated in single ion storage mode. Under the best conditions, the enrichment factors and extraction recoveries were in the range of 113–124 and 74–103%, respectively. The limits of detection were between 3 and 15 ng/L, and the relative standard deviations were < 10%. This method was successfully used for the determination of organophosphorus pesticides in dam water, lagoon water, and river water samples with good reproducibility and recovery.
Keywords:Large volume injection  Magnetic multiwalled carbon nanotubes  Organophosphorus pesticides
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