色谱Issue(7):723-729,7.DOI:10.3724/SP.J.1123.2014.03023
聚酰胺固相萃取-超高效液相色谱-串联质谱法同时检测饲料中的6种全氟化合物
Simultaneous determination of six perfluorinated organic compounds in feed by using polyamide solid-phase extraction with ultra performance liquid chromatography-tandem mass spectrometry
摘要
Abstract
A method for the determination of six perfluorinated organic compounds( PFCs)in feed has been developed. It is based on polyamide solid-phase extraction( SPE)together with ultra performance liquid chromatography-tandem mass spectrometry ( UPLC-MS/MS ). The sample was extracted by acidified acetonitrile. The extraction solution was enriched by a poly-amide SPE cartridge under acidic condition,and cleaned-up using methanol,eluted by 5%( v/v)ammonia/methanol solvent and determined by UPLC-MS/MS. The UPLC separation was carried out on an Acquity BEH C18 column(100 mm×2. 1 mm,1. 7 μm). The mobile phases were 5 mmol/L ammonium acetate and acetonitrile with a gradient elution. Under the optimal conditions,the PFCs were analyzed under multiple reaction monitoring( MRM)mode with neg-ative electrospray ionization. The isotope internal standard method was used to determine the six PFCs,and improve the quantitative accuracy. All of the target compounds exhibited good linearity( r﹥0. 995)over a concentration range of 0. 5-25 μg/L. The detection limits of the six PFCs were all smaller than 0. 1 μg/kg. The mean recoveries of the six PFCs were in the range of 94. 2% to 108. 9% with the relative standard deviations( RSDs)of 1. 8%-8. 6%( n=6). The method for the determination of PFCs in feed is low-cost,favorable effect and suitable for the detection of complex matrix samples.关键词
聚酰胺固相萃取/超高效液相色谱-串联质谱/全氟有机化合物/饲料Key words
polyamide solid-phase extraction/ultra performance liquid chromatography-tandem mass spectrometry( UPLC-MS/MS)/perfluorinated organic compounds( PFCs)/feed分类
化学化工引用本文复制引用
林钦,付凤富,陈国南,郑小严,戴明..聚酰胺固相萃取-超高效液相色谱-串联质谱法同时检测饲料中的6种全氟化合物[J].色谱,2014,(7):723-729,7.基金项目
国家质量监督检验检疫总局科技计划项目(2012QK029). ()