Analysis of Cyromazine in Poultry Feed Using the QuEChERS Method Coupled with LC-MS/MS^†

Abstract

Cyromazine is used as an additive in poultry feed to inhibit the development of fly larvae in chicken manure. U.S. Environmental Protection Agency (EPA) method AG-555, modified from method AG-376, has been the standard method for cyromazine analysis in poultry feed. However, these methods are time-consuming ( approximately 3 h) and require large volumes (200 mL) of solvent. This study developed an extraction procedure using the QuEChERS method that is faster ( approximately 30 min) and uses 20 times less solvent than the AG-555 method. After extraction using the QuEChERS method, the extractant was subjected to cleanup using a C-18 solid phase extraction (SPE) followed by filtering through a 0.45 microm syringe Teflon filter before the liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis. Recovery of 75.0 +/- 6.2% was achieved. The method detection limit (MDL) and the limit of quantitation (LOQ) were 0.028 and 0.094 ppm, respectively. Analyses of commercial poultry feed samples using the QuEChERS method yielded results similar to those obtained via EPA method AG-555.

Cyromazine Determination in Poultry based Animal Feedstuffs by HPLC/DAD using QuEChERS Methodology

“…Recovery of 75.0 ± 6.2% was achieved. The method detection limit and the limit of quantitation were 0.028 and 0.094 ppm, respectively [13].…”

“…With regards to melamine and cyromazine in animal feed there are several studies for their simultaneous determination or single analyte methods. The Quick Easy Cheap Effective Rugged Safe (QuEChERS) approach for cyromazine has been applied only in one paper [13].…”

O estado da arte na determinação de resíduos de medicamentos veterinários em alimentos de origem animal empregando técnicas cromatográficas acopladas à espectrometria de massas

“…70 Inicialmente desenvolvido para ser aplicado na extração de resíduos de agrotóxicos em alimentos de origem vegetal, vem ganhando espaço também na análise de resíduos de medicamentos veterinários em alimentos de origem animal. [71][72][73] O método QuEChERS envolve as seguintes etapas: extração (agitação manual ou mecânica da amostra e acetonitrila (geralmente na proporção 1:1); partição: adição de sais para promover o efeito salting out, o tamponamento do pH do meio, além da remoção de água) e limpeza do extrato (realizada por extração em fase sólida dispersiva (dispersive solid phase extraction, D-SPE). 69 A extração em tubo fechado possui as vantagens de possibilitar a extração em campo e evitar a necessidade de lavagem do homogeneizador entre as extrações.…”

Cyromazine imprinted polymers for selective stir bar sorptive extraction of melamine in animal feed and milk samples

“…4,5 In recent years, melamine with high nitrogen content (66.7%) has been found to be used illicitly as food additive to artificially increase the apparent protein levels of dairy products, which are generally quantified by Kjeldahl method based on the measurement of total nitrogen content. High-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), 8,9 HPLC-diode array detection (DAD) 10,11 and gas chromatography (GC)-MS 12 have been widely employed for the analysis of melamine in different samples. Therefore, reliable and sensitive methods are needed to determine melamine residues in food, particularly in dairy products for children, which is of biological, clinical and food industrial importance.…”