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Method validation for the analysis of 169 pesticides in soya grain, without clean up, by liquid chromatography-tandem mass spectrometry using positive and negative electrospray ionization.
J Chromatogr A. 2007 Feb 23; 1142(2):123-36.JC

Abstract

Part of a comprehensive study on the comparison of different extraction methods, GC-MS(/MS) and LC-MS/MS detection methods and modes, for the analysis of soya samples is described in this paper. The validation of an acetone-based extraction method for analysis of 169 pesticides in soya, using LC-MS/MS positive and negative electrospray ionisation (ESI) mode, is reported. Samples (5 g) were soaked with 10 g water and subsequently extracted with 100 mL of a mixture of acetone, dichloromethane and light petroleum (1:1:1), in the presence of 15 g anhydrous sodium sulphate. After centrifugation, aliquots of the extract were evaporated and reconstituted in 1.0 mL of methanol, before direct injection of the final extract (corresponding with 0.05 g soya mL(-1)) into the LC-MS/MS system. Linearity, r(2) of calibration curves, instrument limit of detection/quantitation (LOD/LOQ) and matrix effect were evaluated, based on seven concentrations measured in 6-fold. Good linearity (at least r(2)> or =0.99) of the calibration curves was obtained over the range from 0.1 or 0.25 to 10.0 ng mL(-1), corresponding with pesticide concentrations in soya bean extract of 2 or 5-200 microg kg(-1). Instrument LOD values generally were 0.1 or 0.25 ng mL(-1). Matrix effects were negligible for approximately 90% of the pesticides. The accuracy, precision and method LOQ were determined via recovery experiments, spiking soya at 10, 50, 100 microg kg(-1), six replicates per level. In both ESI modes, method LOQ values were mostly 10 or 50 microg kg(-1) and more than 70% of pesticides analysed by each mode met the acceptability criteria of recovery (70-120%) and RSD (< or =20%), at one or more of the three levels studied. A fast, easy and efficient method with acceptable performance was achieved for a difficult matrix as soya, without cleanup.

Authors+Show Affiliations

Federal University of Santa Maria, Chemistry Department, Laboratory of Pesticide Residues Analysis (LARP), Santa Maria, RS, Brazil.No affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't
Validation Study

Language

eng

PubMed ID

17222861

Citation

Pizzutti, Ionara R., et al. "Method Validation for the Analysis of 169 Pesticides in Soya Grain, Without Clean Up, By Liquid Chromatography-tandem Mass Spectrometry Using Positive and Negative Electrospray Ionization." Journal of Chromatography. A, vol. 1142, no. 2, 2007, pp. 123-36.
Pizzutti IR, de Kok A, Zanella R, et al. Method validation for the analysis of 169 pesticides in soya grain, without clean up, by liquid chromatography-tandem mass spectrometry using positive and negative electrospray ionization. J Chromatogr A. 2007;1142(2):123-36.
Pizzutti, I. R., de Kok, A., Zanella, R., Adaime, M. B., Hiemstra, M., Wickert, C., & Prestes, O. D. (2007). Method validation for the analysis of 169 pesticides in soya grain, without clean up, by liquid chromatography-tandem mass spectrometry using positive and negative electrospray ionization. Journal of Chromatography. A, 1142(2), 123-36.
Pizzutti IR, et al. Method Validation for the Analysis of 169 Pesticides in Soya Grain, Without Clean Up, By Liquid Chromatography-tandem Mass Spectrometry Using Positive and Negative Electrospray Ionization. J Chromatogr A. 2007 Feb 23;1142(2):123-36. PubMed PMID: 17222861.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Method validation for the analysis of 169 pesticides in soya grain, without clean up, by liquid chromatography-tandem mass spectrometry using positive and negative electrospray ionization. AU - Pizzutti,Ionara R, AU - de Kok,André, AU - Zanella,Renato, AU - Adaime,Martha B, AU - Hiemstra,Maurice, AU - Wickert,Cristine, AU - Prestes,Osmar D, Y1 - 2007/01/12/ PY - 2006/11/03/received PY - 2006/12/04/revised PY - 2006/12/05/accepted PY - 2007/1/16/pubmed PY - 2007/3/27/medline PY - 2007/1/16/entrez SP - 123 EP - 36 JF - Journal of chromatography. A JO - J Chromatogr A VL - 1142 IS - 2 N2 - Part of a comprehensive study on the comparison of different extraction methods, GC-MS(/MS) and LC-MS/MS detection methods and modes, for the analysis of soya samples is described in this paper. The validation of an acetone-based extraction method for analysis of 169 pesticides in soya, using LC-MS/MS positive and negative electrospray ionisation (ESI) mode, is reported. Samples (5 g) were soaked with 10 g water and subsequently extracted with 100 mL of a mixture of acetone, dichloromethane and light petroleum (1:1:1), in the presence of 15 g anhydrous sodium sulphate. After centrifugation, aliquots of the extract were evaporated and reconstituted in 1.0 mL of methanol, before direct injection of the final extract (corresponding with 0.05 g soya mL(-1)) into the LC-MS/MS system. Linearity, r(2) of calibration curves, instrument limit of detection/quantitation (LOD/LOQ) and matrix effect were evaluated, based on seven concentrations measured in 6-fold. Good linearity (at least r(2)> or =0.99) of the calibration curves was obtained over the range from 0.1 or 0.25 to 10.0 ng mL(-1), corresponding with pesticide concentrations in soya bean extract of 2 or 5-200 microg kg(-1). Instrument LOD values generally were 0.1 or 0.25 ng mL(-1). Matrix effects were negligible for approximately 90% of the pesticides. The accuracy, precision and method LOQ were determined via recovery experiments, spiking soya at 10, 50, 100 microg kg(-1), six replicates per level. In both ESI modes, method LOQ values were mostly 10 or 50 microg kg(-1) and more than 70% of pesticides analysed by each mode met the acceptability criteria of recovery (70-120%) and RSD (< or =20%), at one or more of the three levels studied. A fast, easy and efficient method with acceptable performance was achieved for a difficult matrix as soya, without cleanup. SN - 0021-9673 UR - https://www.unboundmedicine.com/medline/citation/17222861/Method_validation_for_the_analysis_of_169_pesticides_in_soya_grain_without_clean_up_by_liquid_chromatography_tandem_mass_spectrometry_using_positive_and_negative_electrospray_ionization_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0021-9673(06)02343-0 DB - PRIME DP - Unbound Medicine ER -