Multiresidue pesticide analysis of fruits by ultra-performance liquid chromatography tandem mass spectrometry

Abstract

Ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS-MS) has been used for screening and quantification of 32 pesticides and metabolites in two fruit matrices. The compounds investigated belonged to different chemical families of insecticides, acaricides, fungicides, and herbicides; several metabolites were also included. Quantification was conducted using matrix-matched standards calibration; response was a linear function of concentration in the range tested (10-500 ng mL(-1)). The method was validated with blank samples of lemon and raisin spiked at 0.01 and 0.1 mg kg(-1), and recoveries were satisfactory, between 70 and 110%, for most of the pesticides tested and relative standard deviations were below 15% (n = 5 at each spiking level). Excellent sensitivity resulted in limits of detection for all compounds well below 0.01 mg kg(-1), with the limit of quantification being validated at 0.01 mg kg(-1). The UPLC system generates narrow peaks (approx. 5 s), thus increasing peak height and improving sensitivity. This improved separation efficiency facilitates adequate resolution not only of the analytes but also of matrix interferences compared with conventional HPLC. The method developed could also resolve some geometric isomers. The main advantage of this approach is the high sample throughput achieved because of the short analysis time, which enables satisfactory separation of all the compounds in less than 5 min per sample.

Current mass spectrometry strategies for the analysis of pesticides and their metabolites in food and water matrices

“…In another direct comparison for the determination of 16 pesticides and transformation products in baby foods, UPLC yielded enhanced S/N ratios, narrower peaks and decreased analysis times over HPLC (Leandro et al, 2006). UPLC-QqQ-MS in multi-residue analysis of pesticides aims to increase the number of monitored compounds, reduce the time of the LC separation step and improve the performance characteristics of the determination step (Lambropoulou & Albanis, 2007;Leandro et al, 2007b;Pozo et al, 2007;Gervais et al, 2008;Kovalczuk et al, 2008;Marín et al, 2009;Mol et al, 2008;Taylor et al, 2008;Wang & Leung, 2009). More than 50 pesticides have been determined in alcoholic beverages by UPLC-QqQ-MS in a run time of 11 min acquiring two transitions per analyte (Plaza Bolãnos et al, 2008) while 90 pesticides have been determined in fruit juices by UPLC-QqQ-MS in MRM mode, in the same run time of 11 min (Romero-González, .…”

Rapid and Sensitive Analysis of Eight Polyphenols in Tobacco by Rapid Resolution Liquid Chromatogarphy

“…Currently, the smaller stationary phase particles (<2.0 μm), new bridging structure of stationary phase and high-pressure systems are commercially available. Using this new rapid resolution liquid chromatography (RRLC) technique, higher linear velocity, faster run time, higher sensitivity and resolution are achieved [13][14][15]. Thus, the aims of the present work are 1) to develop a practical extraction and clean-up procedure prior to the analysis of eight polyphenols ( Figure 1) in tobacco; 2) to develop a rapid and sensitive method to the analysis of eight polyphenols; and 3) to determine the polyphenols in actual tobacco samples by the developed RRLC.…”

Amperometric Biosensor for Pesticide Methamidophos Assay

“…Widely available techniques are based on mass spectrometry and/or liquid chromatography (6,15). Biosensors could be an alternative to the classical analytical methods.…”