A QuEChERS-HPLC-MS/MS Method with Matrix Matching Calibration Strategy for Determination of Imidacloprid and Its Metabolites in Procambarus clarkii (Crayfish) Tissues

• Published in: Molecules (Basel, Switzerland) Vol. 26; no. 2; p. 274
• Main Authors: Yang, Qiuhong, Ai, Xiaohui, Dong, Jing, Liu, Yongtao, Zhou, Shun, Yang, Yibin, Xu, Ning
• Format: Journal Article
• Language: English
• Published: Switzerland MDPI AG 07.01.2021; MDPI
• Subjects: 5-hydroxy imidacloprid; Acetic acid; Acetonitrile; Aluminum oxide; Calibration; Cephalothorax; Chromatography; Crayfish; High performance liquid chromatography; HPLC-MS/MS; Imidacloprid; Insecticides; Intestine; Liquid chromatography; Mass spectrometry; Mass spectroscopy; Metabolites; Muscles; Negative ions; Neurotoxicity; olefin imidacloprid; Pesticides; Procambarus clarkii; Quadrupoles; QuEChERS; Solvents; Standard deviation; Tissues; Urea; China; 5-hydroxy imidacloprid; HPLC-MS/MS; Imidacloprid urea; Metabolites; QuEChERS; olefin imidacloprid; Imidacloprid; Procambarus clarkii; 6-chloronicotinic acid
• ISSN: 1420-3049; 1420-3049
• DOI: 10.3390/molecules26020274

We developed a method for determination of imidacloprid and its metabolites 5-hydroxy imidacloprid, olefin imidacloprid, imidacloprid urea and 6-chloronicotinic acid in (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 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 , the limits of quantification were 0.05-2.0 μg·L and the method of quantification was 0.05-2.0 μg·kg . The method is rapid, simple, sensitive and suitable for rapid determination and analysis of imidacloprid and its metabolites in tissues.