Metal organic frameworks are considered as an efficient and promised adsorbent for separation of several ions and compounds from solutions due to its unique geometric structure. Herein, copper‐benzyl tricarboxylic acid based metal organic frameworks have showed a high efficiency in enrichment and microextraction of malathion from food and water samples. The microextraction procedures were followed by determination of malathion by ultra high performance liquid chromatography with tandem mass spectrometry. The optimum recoveries for malathion were obtained at pH 6, and with using 2 mL of ethyl acetate as the eluent. The microextraction procedures showed a detection limits and the quantification limits of 4.0 and 10.0 µg/L, respectively. The intra‐ and interday precision showed a relative standard deviation% less than 10. The feasibility of the proposed procedure was determined by evaluating the addition/recovery studies of malathion from the real samples. The absolute recovery% was ≥92%. Furthermore, some ions were tested as cointerfering ions, and the recovery% was 93‐100%. These results confirm that the developed microextraction procedure based on copper‐benzyl tricarboxylic acid based metal organic frameworks as extractor for dispersive solid phase microextraction is matrix‐independent, and can be applied for various real samples including different matrix or various malathion content.
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