Determination of Botanical Insecticides Residues in Fish by Liquid Chromatography–Electrospray Tandem Mass Spectrometry

Abstract

A method for determining residues of four botanical insecticides oxymatrine, matrine, rotenone, and azadirachtin in fish by liquid chromatographyelectrospray tandem mass spectrometry (LC-MS/MS) is described. The extraction was achieved using acetonitrile, with the addition of sodium chloride to induce a salting out effect before using n-hexane to defat. Chromatographic separation is achieved on Phenomenex Luna C18 column in the mobile phase composition of acetonitrile and 5 mmol/L ammonium acetate buffer consisting formic acid to provide protons for LC-MS/ MS analysis. Accomplishing with the matrix matched calibration curves to compensate for the matrix effect, the quantitative data showed good linear response within the concentration ranges studied. Detection is carried out using positive-ion electrospray tandem mass spectrometry. Calibrations were linear over a working range of 0.5-50 μg/L for oxymatrine, matrine, rotenone, and 2-200 μg/L for azadirachtin. The average recoveries and the relative standard deviation ranged from 88.6-95.7% and 7.58-10.2%, respectively, in spiked fish samples at concentration levels ranging from 0.5 to 10 μg/kg for oxymatrine, matrine, and rotenone and from 2 to 50 μg/kg for azadirachtin. The limits of detection for oxymatrine, matrine, rotenone, and azadirachtin were 0.29, 0.37, 0.21, and 1.4 μg/kg, respectively. The method is accurate, specific, and sensitive for the analysis of the studied botanical insecticides residues in fish samples.

Simultaneous determination of five azadirachtins in the seed and leaf extracts of Azadirachta indica by automated online solid-phase extraction coupled with LC–Q-TOF–MS

“…Sample extraction was based on the previous study with some modifications [ 21 ]. A portion (0.10 g) of well-homogenized powdered leaves or seeds was weighted in a 40 mL glass bottle.…”

Synthesis of Halopyrazole Matrine Derivatives and Their Insecticidal and Fungicidal Activities

“…Plant pests and diseases not only endanger food security and reduce food quality but also affect farmers’ income [ 1 ]. The promotion of organic pesticide use has significantly increased grain output, but it has also caused a series of problems such as environmental pollution, food safety and drug resistance [ 2 ]. The development of new green pesticides with high efficiency, low toxicity and easy degradation has become the current development trend.…”

Semi‐synthesis and characterization of some new matrine derivatives as insecticidal agents

“…The developmental trend of pesticides is currently shifting to high efficiency, low toxicity, low residue, and environmentally green. Botanical insecticides with a toxic effect on insects are environmental friendly and easy to degrade, and therefore have become a hot spot in the development of green pesticides, such as matrine, azadirachtin, rotenone, and pyrethrins.…”