摘要
建立了固相萃取-高效液相色谱-串联质谱(HPLC-MS/MS)测定蜂蜜中泰妙菌素残留量的分析方法。样品用甲醇-偏磷酸水溶液提取,OasisMCX SPE小柱净化,经C18色谱柱分离,以电喷雾离子源在正离子多反应监测(MRM)模式下进行测定,外标法定量。泰妙菌素的方法检出限为0.04μg/kg,定量下限为0.1μg/kg,在0.5～50μg/L范围内线性关系良好,相关系数r为0.999 8。在0.1～5.0μg/kg加标水平内泰妙菌素的回收率为80%～94%,RSD为4.5%～8.1%。该方法实用、准确、灵敏,适用于蜂蜜中泰妙菌素残留量的测定。
A method was developed for the determination of tiamulin residues in honey by solid-phase extraction - liquid chromatography - tandem mass spectrometry （ HPLC - MS/MS）. The sample was extracted with methanol- metaphosphoric acid solution, cleaned up by solid phase extraction （SPE） using an oasis MCX extraction catridge. The extract was analyzed by HPLC -MS/MS with a C18 column as analytical column under multiple reaction monitoring（MRM） mode via positive electrospray ionization. The limit of deteciton for tiamulin was 0.04 μg/kg, and the limit of quantitation was 0. 1 μg/kg in honey. The calibration curve had a good linearity from 0.5 μg/L to 50. 0 μg/L with a correlation coefficient of 0. 999 8. The recoveries of tiamulin at spiked levels in the range of 0. 1 - 5.0 μg/kg were 80% -94% with relative standard deviations of 4.5% -8.1%. The method was practi- cal, accurate and sensitive, and was suitable for the determination of tiamulin residues in hoeny sample.
出处
《分析测试学报》
CAS
CSCD
北大核心
2010年第11期1203-1206,共4页
Journal of Instrumental Analysis
关键词
液相色谱-串联质谱
固相萃取净化
蜂蜜
泰妙菌素
残留
liquid chromatography - tandem mass spectrometry（ HPLC - MS/MS）
solid-phase extraction clean up
honey
tiamulin
residues
