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.pdfVIP

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

林钦;付凤富;陈国南;郑小严;戴明

【摘要】Amethodforthedeterminationofsixperfluorinatedorganic

compounds(PFCs)infeedhasbeendeveloped.Itisbasedonpolyamide

solid-phaseextraction(SPE)togetherwithultraperformanceliquid

chromatography-tandemmassspectrometry(UPLC-MS/MS).Thesample

wasextractedbyacidifiedacetonitrile.Theextractionsolutionwas

enrichedbyapoly-amideSPEcartridgeunderacidiccondition,and

cleaned-upusingmethanol,elutedby5%(v/v)ammonia/methanolsolvent

anddeterminedbyUPLC-MS/MS.TheUPLCseparationwascarriedouton

anAcquityBEHC18column(100mm×2.1mm,1.7μm).Themobilephases

were5mmol/Lammoniumacetateandacetonitrilewithagradientelution.

Undertheoptimalconditions,thePFCswereanalyzedundermultiple

reactionmonitoring(MRM)modewithneg-ativeelectrosprayionization.

Theisotopeinternalstandardmethodwasusedtodeterminethesix

PFCs,andimprovethequantitativeaccuracy.Allofthetargetcompounds

exhibitedgoodlinearity(r﹥0.995)overaconcentrationrangeof0.5-25

μg/L.ThedetectionlimitsofthesixPFCswereallsmallerthan0.1μg/kg.

ThemeanrecoveriesofthesixPFCswereintherangeof94.2%to108.9%

withtherelativestandarddeviations(RSDs)of1.8%-8.6%(n=6).The

methodforthedeterminationofPFCsinfeedislow-cost,favorableeffect

andsuitableforthedetectionofcomplexmatrixsamples.%建立了饲料中6

种全氟化合物的聚酰胺固相萃取-超高效液相色谱-串联四极杆质谱分析法。样品采

用酸化乙腈提取，在酸性条件下用聚酰胺固相萃取小柱富集，甲醇淋洗净化，5％

（v/v）氨水/甲醇溶液洗脱后采用超高效液相色谱-串联四极杆质谱（UPLC-

MS/MS）检测。分析柱为AcquityBEHC18（100mm×2.1mm，1.7μm）；

流动相为5mmol/L乙酸铵-乙腈梯度洗脱；在最佳实验条件下，采用多反应监测

负离子模式测定，同位素内标法定量。该方法对6种全氟化合物的检出限均小于

0.1μg/kg；对6种饲料及原料的加标回收率为94.2％~108.9％，精密度（RSD）

为1.8％~8.6％（n=6）；在0.5~25μg/L范围内均呈良好的线性关系，线性回

归系数r﹥0.995。该方法前处理成本低，效果好，适合复杂基质样品的检测。

【期刊名称】《色谱》

【年(卷),期】2014(000)007

【总页数】7页(P723-729)

【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;