Determination of residue levels of the avicide 3-chloro-4-methylaniline hydrochloride in red-winged blackbirds (Agelaius phoeniceus) by gas chromatography-tandem mass spectrometry

Authors

David A. Goldade, USDA APHIS Wildlife ServicesFollow
Kirsten R. Kim, USDA APHIS Wildlife Services
James C. Carlson, USDA APHIS Wildlife ServicesFollow
Steven F. Volker, USDA APHIS Wildlife ServicesFollow

Document Type

Article

Date of this Version

2019

Citation

Journal of Chromatography B 1104 (2019) 141–147

Comments

This document is a U.S. government work and is not subject to copyright in the United States.

https://doi.org/10.1016/j.jchromb.2018.11.009

Abstract

The avicide 3‑chloro‑4‑methylanaline hydrochloride (chloro‑p‑toluidine hydrochloride, CPTH, DRC-1339) is used to control pest bird species that damage agricultural crops. A specific and sensitive gas chromatographytandem mass spectrometry method was developed and validated for the determination of CPTH in avian breast muscle, GI tract, kidney, and liver. Tissue samples were extracted with a solution of acidified water and acetonitrile. The sample was made basic and cleaned up with a combination of liquid-liquid partitioning and solid phase extraction. Separation was achieved using a HP-5 ultra-inert GC column (15 M, 0.25 μm film) with detection on a triple quadrupole mass spectrometer in multiple reaction monitoring (MRM) mode. The monitored transition for CPTH was m/z 140.9→106.2 for quantitation and 139.9→105.2 and 139.9→77.2 for confirmation. The linear range was 5 to 5000 ng/mL. The precision for the determination of CPTH in all tissues averaged 7.2% and the accuracy averaged 6.7%. The recovery of CPTH fortified at 5 different levels averaged 101% in liver, 98.8% in GI tract, 92.9% in breast muscle, and 87.9% in kidney. The established method was successfully used to determine CPTH residue levels in red-winged blackbirds exposed to three different doses of CPTH.