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1、2018年12月Vol.36No.12December2018ChineseJournalofChromatography1279~1283研究論文DOI:10.3724/SP.J.1123.2018.07011液相色譜?串聯(lián)質(zhì)譜法同時(shí)測(cè)定嬰幼兒配方乳粉中全氟辛酸、全氟辛烷磺酸、雙酚A和壬基酚殘留?王浩,邵明媛,賈婧怡,劉明艷,裴帆(國(guó)家食品質(zhì)量安全監(jiān)督檢驗(yàn)中心,北京100094)摘要:建立了嬰幼兒配方乳粉中全氟辛酸、全氟辛烷磺酸、雙酚A和壬基酚多殘留的高效液相色譜?串聯(lián)四極桿質(zhì)譜聯(lián)用測(cè)定方法。樣品用水超聲
2、溶解,乙腈沉淀蛋白質(zhì),液相色譜?串聯(lián)質(zhì)譜測(cè)定,基質(zhì)內(nèi)標(biāo)法定量。以HypersilGOLDC色譜柱(50mm×4?6mm,1?9μm)分離,流動(dòng)相為30mmol/L乙酸銨水溶液和甲醇,流速0?3018mL/min。在該優(yōu)化條件下,全氟辛酸、全氟辛烷磺酸、雙酚A和壬基酚的定量限分別為0?5、1?0、10?0和5?0μg/kg,方法回收率為86?1%~106?8%,相對(duì)標(biāo)準(zhǔn)偏差為2?87%~9?53%。測(cè)定了多種市售嬰幼兒配方奶粉,表明該方法操作簡(jiǎn)單、測(cè)定結(jié)果準(zhǔn)確,可用于嬰幼兒配方奶粉中全氟辛酸、全氟辛烷磺酸、雙
3、酚A和壬基酚多殘留的同時(shí)快速測(cè)定。關(guān)鍵詞:液相色譜?串聯(lián)質(zhì)譜;全氟辛酸;全氟辛烷磺酸;雙酚A;壬基酚;嬰幼兒配方乳粉中圖分類號(hào):O658文獻(xiàn)標(biāo)識(shí)碼:A文章編號(hào):1000?8713(2018)12?1279?05Simultaneousdeterminationofperfluoricacid,perfluorooctanesulfonicacid,bisphenolA,nonylphenolininfantmilkpowderbyhigh?performanceliquidchromatography?ta
4、ndemmassspectrometry?WANGHao,SHAOMingyuan,JIAJingyi,LIUMingyan,PEIFan(ChinaNationalFood&SafetySupervisionandInspectionCenter,Beijing100094,China)Abstract:Arapidconfirmativemethodwasdevelopedfordeterminingtheresiduesofperflu?oricacid(PFOA),perfluorooctanesu
5、lfonicacid(PFOS),bisphenolA(BPA),andnonylphe?nol(NP)ininfantmilkpowderbyHPLC?MS/MS.Thesamplewasdissolvedinwaterbyultra?sonication,andtheproteinwasremovedbydissolvinginacetonitrile.Theanalytesweresepa?ratedonaHypersilGOLDCcolumn(150mm×2?0mm,5μm)using30mmol/
6、Lammonium18acetatesolutionandmethanolasmobilephases,withgradientelutionataflowrateof0?3mL/min.Finally,thesamplesweredeterminedbyHPLC?MS/MS.Internalmatrix?matchedcali?brationwasusedforquantification.Thelimitsofquantification(LOQs,S/N=10)ofPFOA,PFOS,BPA,andN
7、Pwere0?5,1?0,10?0,and5?0μg/kg,respectively.Therecoveriesrangedfrom86?1%to106?8%,andtherelativestandarddeviations(RSDs)wereintherangefrom2?87%to9?53%.Themethodwasalsoappliedtorealsamples.Theresultsshowedthatthemethodwassimpleandaccurate,andcanbeusedfordeter
8、miningtheresiduesofPFOA,PFOS,BPA,andNPininfantmilkpowder.Keywords:high?performanceliquidchromatographytandemmassspectrometry(HPLC?MS/MS);perfluoricacid(PFOA);perfluorooctanesulfonicacid(PFOS);bisphenolA(BPA);