A Simple and Selective Method for the Measurement of Azadirachtin and Related Azadirachtoid Levels in Fruits and Vegetables Using Liquid Chromatography Electrospray Ionization Tandem Mass Spectrometry

Abstract

Neem-based insecticides containing azadirachtin and related azadirachtoids are widely used in agriculture. Here, we report an analytical method for the rapid and accurate quantification of the insecticide azadirachtin A and B and other azadirachtoids such as salannin, nimbin, and their deacetylated analogues on tomatoes and peaches. Azadirachtoids were extracted from fruits and vegetables with acetonitrile. Using high-performance liquid chromatography/electrospray ionization tandem mass spectrometer, azadirachtoids were selectively detected monitoring the multiple reaction transitions of sodium adduct precursor ions. For azadirachtin A, calibration was linear over a working range of 1-1000 microg/L with r > 0.996. The limit of detection and limit of quantification for azadirachtin A were 0.4 and 0.8 microg/kg, respectively. The presence of interfering compounds in the peach and tomato extracts was evaluated and found to be minimal. Because of the linear behavior, it was concluded that the multiple reaction transitions of sodium adduct ions can be used for analytical purposes, that is, for the identification and quantification of azadirachtin A and B and related azadirachtoids in fruit and vegetable extracts at trace levels.

Antiangiogenic Effects and Therapeutic Targets ofAzadirachta indicaLeaf Extract in Endothelial Cells

“…The scan range for data acquisition was 250–1200  m / z range. The formation of an even electron sodium adduct in the source was utilized to provide increased selectivity for the tetranortriterpenoids [20] present in the EENL.…”

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

“…In the development of large-scale multi-residue methods, a compromise is required that will provide acceptable recoveries for the largest number of analytes and, for this purpose, solvents of medium polarity are commonly selected for SE. Among these solvents, acetonitrile (Kovalczuk et al, 2006;Hengel & Miller, 2007, 2008Caboni et al, 2008;Sarais et al, 2008) ethyl acetate, used in conjunction with anhydrous sodium sulfate (Goto et al, 2006b;Banerjee et al, 2007;Mol et al, 2007;Pan, Xia, & Liang, 2008;Schurek et al, 2008a), methanol (García-Reyes, Stahnke, Reemtsma, & Alder, 2009), acetone (Kuster, López de Alda, & Barceló, 2006;Grimalt et al, 2007), and dichloromethane (Venkateswarlu et al, 2007;Tokman et al, 2009) or mixtures of solvents Pang et al, 2006b) are suitable universal solvents for SE. The SE treatment is occasionally performed with ultrasonication to increase the extraction yield and increase the speed of the procedure (Pan, Xia, & Liang, 2008).…”

“…Approximately 60% of the methodologies reviewed in the present article covering the last 3 years are based on LC-QqQ-MS. Even though the majority of methodologies proposed in the field of pesticide residue-analysis focus on the development of multi-residue multi-class methods using LC-QqQ-MS, several deal with single-residue and/or single-class applications especially in cases where the definition of the residue in the MRL (Commission Regulations (EC), 396/2005, 149/2008, 839/2008 encompass metabolites and transformation products of the parent compound (Goto et al, 2006b;Soler et al, 2006a;Barceló & Petrovic, 2007;Hengel & Miller, 2007;Perreau et al, 2007;Poulsen et al, 2007;Sannino, 2007;Caboni et al, 2008;Crnogorac, Schmauder, & Schwack, 2008;Hayama & Takada, 2008;Hanke, Singer, & Hollender, 2008;Koesukwiwat, Sanguankaew, & Leepipatpiboon, 2008;Sarais et al, 2008;Xinyi et al, 2008;Esparza, Moyano, & Galceran, 2009;Tokman et al, 2009). Nowadays, parent compounds and their transformation products can be analyzed with LC-QqQ-MS in the same chromatographic run; this is especially helpful for official and/or routine laboratories.…”

Comparison of several extraction procedures for the determination of biopesticides in soil samples by ultrahigh pressure LC‐MS/MS

“…Among these compounds, azadirachtin is obtained from neem tree ( Azadirachta indica ) and it is a potent antifeedant to many insects []. Spinosad is originally isolated from the soil Actinomycete bacterium, Saccharopolyspora spinosa [].…”