Determination of antimycin–a in a liquid formulation by high performance liquid chromatography–mass spectrometry

Pesticide formulations containing the active ingredient antimycin–a (ANT–A) have been used by fisheries and aquaculture managers for several decades to remove nuisance fish species. Analytical methods for measuring ANT–A during pesticide treatments have been done using high performance liquid chromatography (HPLC) paired with multiple detection methods (for example, electrochemical, ultraviolet, fluorescence, mass spectrometry). However, instruments and analytical chemistry methods can advance over time because of the need to develop timely, reliable, cost effective, and reproducible methods. Subsequently, ANT–A analytical chemistry methods and sample processing techniques also have improved over the past several decades. In the present study, we describe a liquid chromatography–mass spectrometry method and its verification across three analysts. Each analyst group created a single calibration curve and verified ANT–A in a liquid formulation using the averaged total response of all major ANT–A homologs (A1, A3, A3, A4). The advantage of this technique is that it creates a more resilient ANT–A quantification method amendable to batch-batch differences in major homologs. The method demonstrated how ANT–A can be effectively measured with high accuracy (98–99 percent), precision (2.7–16.2 percent), and specificity within a pesticide liquid formulation using a method applicable for Federal registration requirements.