ABSTRACT
A determination method of nosiheptide in formula feeds by HPLC-FL was developed and validated, including an inter-laboratory study. Formula feeds were extracted with acetone after adding acetic acid. Liquid chromatographic separation was performed using a ZORBAX Eclipse XDB-C18 column, with acetonitrile and water containing acetic acid as the mobile phase. Detection of NH was carried out with a fluorescence detector. Recovery tests and an inter-laboratory study were conducted using chicken and swine formula feeds fortified with nosiheptide at 0.5-27 mg-potency/kg. Mean recoveries in recovery tests ranged from 91.4 to 103%, and the repeatability in terms of relative standard deviation was within 7.8%. Mean recoveries of the inter-laboratory study ranged from 98.4 to 108%, the repeatability and reproducibility in terms of the relative standard deviations were within 8.1% and 13% respectively, and the HorRat values ranged from 0.21 to 0.75.
Subject(s)
Animal Feed/analysis , Chromatography, High Pressure Liquid/methods , Food Analysis/methods , Laboratories , Observer Variation , Reproducibility of Results , Thiazoles/analysis , Thiazoles/isolation & purificationABSTRACT
To evaluate a method using a multifunctional clean-up column coupled with high performance liquid chromatography as an official analytical method for the determination of deoxynivalenol in wheat used as food or feed, an inter-laboratory study was performed in 12 laboratories using four naturally contaminated wheat samples and one spiked sample. The relative standard deviations for repeatability (RSDr) and reproducibility (RSDR) of naturally contaminated wheat were in the range 5.8-11.3% and 12.0-20.7%, respectively. The HORRAT was less than 1.0 in each sample. From the spiking test, the recovery rate, RSDr, RSDR and HORRAT value were 100.0%, 11.2%, 10.3% and 0.5, respectively. The limit of quantification is 0.10 mg/kg from the range obtained in a linear calibration. Thus, it should be useful as a sensitive and validated analytical method for the determination of deoxynivalenol in wheat intended for use in food and feed.
