Rapid Method for the Determination of 180 Pesticide Residues in Foods by Gas Chromatography/Mass Spectrometry and Flame Photometric Detection

Abstract

A method was established for the determination of 180 pesticide residues in fruits and vegetables. The procedure involved extraction with acetonitrile, followed by a salting-out step with anhydrous MgSO 4 and NaCl. Removal of sediment and water was performed simultaneously by centrifugation. Co-extractives were removed with a double-layered SPE column, and graphitized carbon black and primary secondary amine (GCB/PSA) solid phase extraction cleanup cartridge. The eluate was determined by GC/FPD and GC/MS without further cleanup. Recovery data were obtained by fortifying 9 matrices at 0.05-0.1 mg/g. Recoveries of 180 pesticides were mainly 70-110% and the relative standard deviation (RSD) was below 25%. Limits of detection ranged between 0.01 and 0.05 mg/g for tested pesticides.

Multi-residue screening method of acidic pesticides in agricultural products by liquid chromatography/time of flight mass spectrometry

“…For the multi-residue method, Lee 11) recommended salting-out at pH 7.0, but currently salting out at weak-acidic pH has been adopted by Anastassiades 7) and Okihashi. 12) If salting-out at pH 5-5.5 was adopted after verifying the applicability for the target pesticides in our multi-residue method, recovery of acidic pesticides would be improved.…”

Rapid and Easy Multiresidue Method for Determination of Pesticide Residues in Foods Using Gas or Liquid Chromatography–Tandem Mass Spectrometry

“…We also examined the QuEChERS method and found that the characteristic points of the method (step (2)) are positive aspects; however, steps (1) and (3) are negative aspects due to the weak extraction potency (shaking) and the insufficient cleanup (dispersive-SPE). To overcome these negative aspects, we developed a new powerful extraction technique with a homogenizer and with an efficient cleanup with double-layered SPE (graphite carbon black (GCB) with PSA) on the basis of the QuEChERS method (Okihashi, M., et al, 2005, Takatori, S., et al, 2008. We demonstrated that this method is applicable to the multiresidue analysis in agricultural products by the combination of analysis with gas chromatography equipped with (tandem) mass spectrometry (GC-MS or GC-MS/MS) and with highperformance liquid chromatography with tandem mass spectrometry (LC-MS/MS).…”

Difference in the matrix components by cleanup methods between the notified multiresidue pesticide analysis method in Japan and the QuEChERS method

“…We also must consider how to react PSA or NH 2 with the fatty acids. Since the combination of the QuEChERS extraction and filled SPE cleanup like Okihashi's 8,9) method has been adopted by many laboratories in Japan, the matrix components using that kind of method need to be investigated in the future. It is also necessary to develop a method to remove the monoacylglycerols in the JPL method.…”

“…Recently, the interest of this simplified method has been increasing in Japan. Okihashi et al 8,9) evaluated its rapid approach; however, concerned about the weak extraction potency and insufficient cleanup, they modified the QuEChERS method.…”