Determination of 5 Quinoxaline Residues in Feed by On-line Solid Phase Extraction/Liquid Chromatography-Tandem Mass Spectrometry Method[J]. 2015,34(5):610-615.
Determination of 5 Quinoxaline Residues in Feed by On-line Solid Phase Extraction/Liquid Chromatography-Tandem Mass Spectrometry Method[J]. 2015,34(5):610-615.DOI:
在线固相萃取/液相色谱-串联质谱法检测饲料中5种喹啉药物残留量
摘要
建立了在线固相萃取/液相色谱-串联质谱法检测饲料中5种喹啉药物的方法。准确称取2 g饲料,用10 mL 0.1%盐酸-甲醇(1∶1)提取,提取液用0.2%甲酸稀释10倍,通过双三元液相色谱采用反相在线固相萃取柱在线富集净化,以0.2%甲酸与乙腈梯度洗脱,同时转移至C18色谱柱上进行分离,串联四极杆质谱检测。实验结果表明,5种喹啉药物在50~25 000 μg/kg含量范围内线性良好(r>0.999);方法的检出限为25 μg/kg,定量下限为50 μg/kg;方法回收率为72.6%~84.6%,批内和批间相对标准偏差(RSD)均小于10%。本方法较传统固相萃取柱净化法更简捷、经济和稳定。
Abstract
A high performance liquid chromatography-tandem mass spectrometric method with on-line SPE(solid phase extraction) was established for the determination of 5 quinoxaline residues in feed.2 g feed was extracted with 10 mL 0.1% HCl-CH3OH(1∶1).The extract was 10 times diluted with 0。2% formic acid.The dissolution was enriched and purified with a reverse phase on-line SPE column on a double ternary liquid chromatograph.Target compounds were eluted with 0.2% formic acid and acetonitrile by gradient elution,and separated with an octadecyl silica bonded column.Target compounds were then determined by tandem mass spectrometry.The results showed that the linearities of 5 quinoxalines were good in the range of 50-25 000 μg/kg(r>0.999).The LOD of the method was 25 μg/kg,and LOQ was 50 μg/kg.Recoveries of 5 quinoxalines were in the range of 72.6%-84.6%,while RSDs of both in the batch and between the batch were all lower than 10%.The method was proved to be more convenient,economical and stable than the traditional column SPE method.
关键词
在线固相萃取双三元液相色谱-串联质谱法喹噁啉类药物饲料
Keywords
on-line SPEdouble ternary liquid chromatography-tandem mass spectrometryquinoxalinesfeed