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

• Published in: Journal of chromatography. B, Analytical technologies in the biomedical and life sciences Analytical technologies in the biomedical and life sciences, 2019-01, Vol.1104, p.141-147
• Main Authors: Goldade, David A., Kim, Kirsten R., Carlson, James C., Volker, Steven F.
• Format: Article
• Language: English
• Subjects: Avicide; CPTH; DRC-1339; GC–MS-MS; Red-winged blackbirds
• ISSN: 1570-0232; 1873-376X
• DOI: 10.1016/j.jchromb.2018.11.009

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 chromatography-tandem 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. •A GC-MS-MS method was validated for the determination of CPTH in avian breast muscle, GI tract, liver, and kidney.•The CPTH recovery at 5 different levels averaged between 87.9 and 101%.•The method was used to determine CPTH residue levels in red-winged blackbirds exposed to three different doses of CPTH.•CPTH was detected in all tissues in birds receiving an oral dose.