高效液相色谱串联静电轨道离子阱质谱筛查奶粉中16种磺胺类药物
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摘要
建立了超高效液相色谱串联高分辨质谱Q-Exactive快速定性筛查婴幼儿奶粉中16种磺胺类药物残留的方法。2 g奶粉样品以6 mL乙腈和4 mL水为溶剂提取,均质震荡后,使用无水硫酸镁脱水,离心后取乙腈层用100 mg C_(18)固相吸附剂净化,并采用针头式滤膜过滤进样。本方法以FullMS/AIF (数据非依赖模式)扫描样品信息,FullMS/ddms2(数据依赖)模式建立包含保留时间、母离子质核比、碎片离子信息的磺胺药物的数据库,利用Tracefinder软件对样品中残留的磺胺类药物进行快速的定性和定量。结果表明,16种磺胺类药物在10,50,100μg/kg添加水平内,平均加标回收率为67%～116%,RSD为1. 8%～12%,在各自的考察浓度范围内线性关系良好,R> 0. 99。
Screening method of 16 sulfonamides residues in infant formula was established by using high performance liquid chromatography coupled with high resolution mass spectrometry Q-exactive.Infant formula( 2 g) was extracted with 6 m L acetonitrile and 4 m L water. After homogenous shock,the solution was dehydrated with anhydrous magnesium sulfate,and the layer of acetonitrile was purified with 100 mg C_(18) after centrifugation. Samples were filtered by needle filter membrane before analysis. Screening information database was established by scanning model of FullMS/AIF and FullMS/ddms2,which contained retention time,mother ion mass ratio,sulfonamide fragment ions.Thus,using Trace Finder software,qualitative and quantitative analysis for sulfonamides residues in samples were achieved efficiently. The results showed that the spiked recoveries were 67%-116%,with RSDs of 1. 8%-12% at the level of 10,50 and 100 μg/kg for 16 sulfonamides.
Screening method of 16 sulfonamides residues in infant formula was established by using high performance liquid chromatography coupled with high resolution mass spectrometry Q-exactive.Infant formula( 2 g) was extracted with 6 m L acetonitrile and 4 m L water. After homogenous shock,the solution was dehydrated with anhydrous magnesium sulfate,and the layer of acetonitrile was purified with 100 mg C_(18) after centrifugation. Samples were filtered by needle filter membrane before analysis. Screening information database was established by scanning model of FullMS/AIF and FullMS/ddms2,which contained retention time,mother ion mass ratio,sulfonamide fragment ions.Thus,using Trace Finder software,qualitative and quantitative analysis for sulfonamides residues in samples were achieved efficiently. The results showed that the spiked recoveries were 67%-116%,with RSDs of 1. 8%-12% at the level of 10,50 and 100 μg/kg for 16 sulfonamides.
引文
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