Analysis of pesticides in fruit, vegetables and cereals using methanolic extraction and detection by liquid chromatography–tandem mass spectrometry

Abstract A method for analysing carbamates and other relatively polar pesticides by LC–MS–MS with electrospray ionisation has been developed. The method is based on extraction by ultrasonication using a methanolic ammonium acetate–acetic acid buffer. After centrifugation the samples are filtered in Miniprep filter HPLC vials and detected by LC–MS–MS. To compensate for variations in the MS response [ 13 C 6 ]-carbaryl was used as internal standard and matrix-matched pesticide solutions were used as external standards for the quantification. The method has been validated for the matrices apple, avocado, carrot, lettuce, orange, potato and wheat at the spiking levels—0.02; 0.04 and 0.20 mg kg−1. Recoveries were generally in the range 70–120%. Results from participation in three intercomparisons proved the accuracy of the method. As the analytical procedure does not include any concentration or cleanup steps, it is easy and fast to perform, making it applicable for routine analysis in large pesticide monitoring programmes.

[1]  M. Poulsen,et al.  Estimation of the uncertainty in a multiresidue method for the determination of pesticide residues in fruit and vegetables , 2003, Food additives and contaminants.

[2]  D. Hercules,et al.  LC-MS/MS signal suppression effects in the analysis of pesticides in complex environmental matrices , 2001, Fresenius' journal of analytical chemistry.

[3]  G. Bordin,et al.  How to overcome matrix effects in the determination of pesticides in fruit by HPLC–ESI–MS–MS , 2001, Fresenius' journal of analytical chemistry.

[4]  W. Niessen,et al.  Determination of pesticides in vegetables using large-volume injection column liquid chromatography-electrospray tandem mass spectrometry. , 2000, Journal of chromatography. A.

[5]  QUALITY CONTROL PROCEDURES FOR PESTICIDE RESIDUES ANALYSIS , 2004 .

[6]  G. G. Stokes "J." , 1890, The New Yale Book of Quotations.

[7]  J. Hajšlová,et al.  Determination of seventeen polar/thermolabile pesticides in apples and apricots by liquid chromatography/mass spectrometry. , 2003, Journal of AOAC International.

[8]  D. Barceló,et al.  Choosing between atmospheric pressure chemical ionization and electrospray ionization interfaces for the HPLC/MS analysis of pesticides. , 2001, Analytical chemistry.

[9]  Anwar Hadi,et al.  Sistem Manajemen Mutu Laboratorium - Sesuai ISO/IEC 17025: 2000 General Requirements for the Competence of Testing and Calibration Laboratories , 2000 .

[10]  Jitka Zrostlíková,et al.  Matrix effects in (ultra)trace analysis of pesticide residues in food and biotic matrices. , 2003, Journal of chromatography. A.

[11]  Y. Picó,et al.  Determination of carbamate residues in fruits and vegetables by matrix solid-phase dispersion and liquid chromatography-mass spectrometry. , 2000, Journal of chromatography. A.

[12]  L. Alder,et al.  Applicability of gradient liquid chromatography with tandem mass spectrometry to the simultaneous screening for about 100 pesticides in crops. , 2003, Journal of AOAC International.

[13]  Stephen L. R. Ellison,et al.  Estimating measurement uncertainty using a cause and effect and reconciliation approachPart 2.† Measurement uncertainty estimates compared with collaborative trial expectation‡ , 1998 .

[14]  J. Startin,et al.  High‐performance Liquid Chromatography/Atmospheric Pressure Chemical Ionization Mass Spectrometry with Ionization Polarity Switching for the Determination of Selected Pesticides , 1997 .

[15]  A. Fajgelj,et al.  Validation of a multi-residue method for analysis of pesticides in fruit, vegetables and cereals by a GC/MS iontrap system , 2000 .