Abstract
We developed a method for determination of imidacloprid and its metabolites 5-hydroxy imidacloprid, olefin imidacloprid, imidacloprid urea and 6-chloronicotinic acid in Procambarus clarkii (crayfish) tissues using quick, easy, cheap, effective, rugged, and safe (QuEChERS) and high-performance liquid chromatography-triple quadrupole mass spectrometry. Samples (plasma, cephalothorax, hepatopancrea, gill, intestine, and muscle) were extracted with acetonitrile containing 0.1% acetic acid and cleaned up using a neutral alumina column containing a primary secondary amine. The prepared samples were separated using reverse phase chromatography and scanned in the positive and negative ion multiple reaction-monitoring modes. Under the optimum experimental conditions, spiked recoveries for these compounds in P. clarkii samples ranged from 80.6 to 112.7% with relative standard deviations of 4.2 to 12.6%. The limits of detection were 0.02–0.5 μg·L−1, the limits of quantification were 0.05–2.0 μg·L−1 and the method of quantification was 0.05–2.0 μg·kg−1. The method is rapid, simple, sensitive and suitable for rapid determination and analysis of imidacloprid and its metabolites in P. clarkii tissues.
Highlights
Procambarus clarkii is a species of freshwater crayfish native to northern Mexico and the southern and southeastern United States and has been introduced into many areas of China [1]
In order to improve the signal strength of 6-chloronicotinic acid, we connected a three-way valve to the ESI source, one side was into the standard solution, the other was into the mobile phase, which could adjust the pH and alter the signal strength
We found 6-chloronicotinic acid showed a better peak with an acidic mobile phase
Summary
Procambarus clarkii is a species of freshwater crayfish native to northern Mexico and the southern and southeastern United States and has been introduced into many areas of China [1]. Imidacloprid (1-6-chloro-3-pyridylmethyl-N-nitroimidazol-2-ylideneamine) is a neurotoxic insecticide of the neonicotinoid family class It has high activity, broad insecticidal spectrum, good system physical properties and field stability. Broad insecticidal spectrum, good system physical properties and field stability This compound is the current pesticide of choice to control sucking insect pests on rice, cotton, wheat, vegetables and fruit trees [4,5,6,7,8]. Numerous detection methods have been established for imidacloprid and its metabolites in animal and plant tissues [14,19,20,21,22] These have included measuring levels of imidacloprid in bees and honey products, pistachio nuts and green tea [12,16]. We examined retail P. clarkii samples for the presence of imidacloprid and its metabolites
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