Determination of apramycin in animal feeds by solid-phase extraction and liquid chromatography with precolumn derivatization and fluorescence detection.
A high-performance liquid chromatographic method for determining apramycin in animal feeds was developed. Apramycin in feeds was extracted with 0.1 M HCl solution and cleaned up with an MCX solid-phase extraction column. The purified extract was derivatized with o-phthaldehyde, and components were separated on a C18 column and detected with a fluorescence detector. Mass spectrometric data confirmed that apramycin was derivatized at all the 4 primary amines on the apramycin molecule. Average recoveries at 8 included levels (5, 10, 20, 40, 80, 200, 400, and 2000 mg/kg) ranged from 92.2 to 100.5%, and the coefficients of variation were < 6.5%. Standard curves were linear over the range 0.05 to 10 microg/mL. The detection and quantitation limits were determined to be 0.2 and 1.0 mg/kg, respectively.
Zhang
Liying
L
China Agricultural University, State Key Laboratory on Animal Nutrition, Beijing 100094, People's Republic of China. zhangly@mafic.ac.cn
Wang
Zongyi
Z
Chang
Biying
B
Yang
Wengjun
W
D000821:Animal Feed; D002021:Buffers; D002626:Chemistry, Pharmaceutical / Q000379:methods; D002853:Chromatography, Liquid / Q000379:methods*; D013058:Mass Spectrometry / Q000379:methods; D008956:Models, Chemical; D009328:Nebramycin / Q000031:analogs & derivatives* / Q000032:analysis / Q000737:chemistry; D015203:Reproducibility of Results; D012821:Silanes / Q000737:chemistry; D052616:Solid Phase Extraction; D013050:Spectrometry, Fluorescence / Q000379:methods*; D013997:Time Factors
D002021:Buffers; D012821:Silanes; D009328:Nebramycin; C024779:octadecylsilane; C011666:apramycin