Determination of Bithionol, Bromophen, Nitroxynil, Oxyclozanide, and Tribromsalan in Milk with Liquid Chromatography Coupled with Tandem Mass Spectrometry

Abstract

Abstract LC/MS/MS was developed to determine the residues of bithionol (BTN), bromofen (BMF), nitroxynil (NTX), oxyclozanide (OCZ), and tribromsalan (TBS) in milk. Samples were extracted with ethyl acetate and cleaned up by liquidliquid separation with acetonitrile and n-hexane. The compounds were determined by RP-LC using a C18 column with 0.1 formic acidmethanol. Mass spectral acquisition was performed in the negative mode by applying selected-reaction monitoring. The method was validated in milk spiked with these compounds at 5600 g/kg; average recoveries were in the range 83.897.1, with RSD values of 1.48.0. The interassay RSDs were less than 11. The LODs of these compounds in milk were 0.1 g/kg. The method was applied to 24 raw milk samples. The concentration of these compounds in all samples was lower than the Japanese maximum residue limits. The method is rapid, sensitive, and specific for monitoring residues of BTN, BMF, NTX, OCZ, and TBS in milk.