title: Microflow liquid chromatography coupled to mass spectrometry--an approach to significantly increase sensitivity, decrease matrix effects, and reduce organic solvent usage in pesticide residue analysis.
abstract: This manuscript reports a new pesticide residue analysis method employing a microflow-liquid chromatography system coupled to a triple quadrupole mass spectrometer (microflow-LC-ESI-QqQ-MS). This uses an electrospray ionization source with a narrow tip emitter to generate smaller droplets. A validation study was undertaken to establish performance characteristics for this new approach on 90 pesticide residues, including their degradation products, in three commodities (tomato, pepper, and orange). The significant benefits of the microflow-LC-MS/MS-based method were a high sensitivity gain and a notable reduction in matrix effects delivered by a dilution of the sample (up to 30-fold); this is as a result of competition reduction between the matrix compounds and analytes for charge during ionization. Overall robustness and a capability to withstand long analytical runs using the microflow-LC-MS system have been demonstrated (for 100 consecutive injections without any maintenance being required). Quality controls based on the results of internal standards added at the samples' extraction, dilution, and injection steps were also satisfactory. The LOQ values were mostly 5 μg kg(-1) for almost all pesticide residues. Other benefits were a substantial reduction in solvent usage and waste disposal as well as a decrease in the run-time. The method was successfully applied in the routine analysis of 50 fruit and vegetable samples labeled as organically produced.
authors.affiliation: Agrifood Campus of International Excellence (ceiA3), European Union Reference Laboratory for Pesticide Residues in Fruit & Vegetables, University of Almeria , Ctra. Sacramento, s/n, 04120 La Cañada de San Urbano, Almerı́a, Spain.
authors.forename: Ana
authors.initials: A
authors.lastname: Uclés Moreno
authors.forename: Sonia
authors.initials: S
authors.lastname: Herrera López
authors.forename: Barbara
authors.initials: B
authors.lastname: Reichert
authors.forename: Ana
authors.initials: A
authors.lastname: Lozano Fernández
authors.forename: María Dolores
authors.initials: MD
authors.lastname: Hernando Guil
authors.forename: Amadeo Rodríguez
authors.initials: AR
authors.lastname: Fernández-Alba
mesh_terms: D002212:Capsicum / Q000737:chemistry; D002853:Chromatography, Liquid / Q000379:methods*; D032084:Citrus sinensis / Q000737:chemistry; D018551:Solanum lycopersicum / Q000737:chemistry; D010573:Pesticide Residues / Q000032:analysis*; D012680:Sensitivity and Specificity; D052616:Solid Phase Extraction / Q000379:methods*; D012997:Solvents / Q000737:chemistry*; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*
chemical_list: D010573:Pesticide Residues; D012997:Solvents