Simultaneous detection of gizzerosine and its precursor histamine in feeds and raw materials using UHPLC–MS/MS to evaluate feed safety risks

Abstract

Gizzerosine is a biogenic amine in feeds with a physiological toxicity 1,000 times that of its precursor, histamine, causing high mortality in poultry. Because feeds containing gizzerosine usually contain high concentrations of histamine, it is of great significance to establish a method for the simultaneous detection of gizzerosine and histamine for feed safety. Herein, we first developed a detection method using 50 % (v/v) acetonitrile(ACN) containing 1 % (v/v) ammonium hydroxide (AH) extraction to synchronously monitor gizzerosine and histamine in feeds and raw materials via UHPLC–MS/MS. Due to the serious positive matrix effect (ME) in existing LC–MS/MS, this study reduced the ME of samples by purifying the extract solution using a mixed-mode cation exchange based solid phase extraction column (MCX-SPE), and simultaneously obtained accurate quantities of 5–500 ng mL−1 gizzerosine and 25–2,500 ng mL−1 histamine. The limit of detection (LOD) values for gizzerosine and histamine were 1.02 ng mL−1 and 3.00 ng mL−1, respectively, which were approximately 390 and 8,000 times more sensitive than the maximum recommended dosage of gizzerosine (0.4 mg kg−1) and limitation standards of histamine (25 mg kg−1) in fish meal, respectively. The samples could only be evaluated in 2 h. The average recoveries of the 6 types of feeds and raw materials ranged from 79.73 % to 110.31 % with a relative standard deviation (RSD) ranging from 1.29 % to 13.35 %. The average recoveries of feeds were generally lower than those of raw materials. Our method was efficient, simple, rapid, accurate, sensitive, and suitable for the simultaneous quantitative analysis of gizzerosine and histamine contents in various feeds, which provided technical support for the quality evaluation of feeds.