Development of a Quantitative Gas Chromatography–Tandem Mass Spectrometry Method for the Determination of Pentobarbital in Dog Food

Abstract

In 2017, a commercially available dog food was found by our laboratory to be adulterated with the euthanasia drug pentobarbital. An FDA class 1 voluntary recall by the company ensued. Since there is no set tolerance for pentobarbital in food or feed, a sensitive method for its detection was required. We describe a simple, yet efficient, method for the extraction and quantitative analysis of the barbiturate in dog food. The procedure relies on a combined food emergency response network (FERN) and QuEChERS (quick, easy, cheap, effective, rugged, and safe) approach to sample extraction followed by quantitative analysis by gas chromatography–tandem mass spectrometry (GC/MS/MS) using pentobarbital-d 5 as an internal standard. This procedure improves upon other GC/MS methodologies in that derivatization of pentobarbital or its deuterated internal standard is unnecessary, and sensitivity to a calculated limit of detection (LOD) of 0.6 ppb and a limit of quantitation (LOQ) of 2 ppb is achieved.

Ultrasound and surfactant‐assisted dispersive liquid–liquid microextraction prior to poly(ethylene oxide)‐mediated stacking in CE for highly sensitive determination of barbiturates in human fluids

“…Various methods have been reported for the determination of barbiturate drugs, such as high-performance liquid chromatography (HPLC) [4,5], gas chromatography (GC) [6,7], capillary electrophoresis (CE) [8], electrochemistry [9], and spectrophotometry [10]. Among these methods, CE offers advantages such as rapid analysis, high resolution, and minimal sample and reagent consumption.…”