中华预防医学杂志
中華預防醫學雜誌
중화예방의학잡지
CHINESE JOURNAL OF
2014年
7期
628-633
,共6页
石瑀%杨琳%李敬光%赵云峰%吴永宁
石瑀%楊琳%李敬光%趙雲峰%吳永寧
석우%양림%리경광%조운봉%오영저
色谱法,液相%串联质谱法%血清
色譜法,液相%串聯質譜法%血清
색보법,액상%천련질보법%혈청
Chromatography,liquid%Tandem mass spectrometry%Serum
目的 建立超高效液相色谱-串联三重四级杆质谱(UPLC-MS/MS)测定血清基质中15种全氟磺酸以及全氟烷酸前体物质的方法.方法 血清中的目标化合物与四丁基铵硫酸氢盐结合后,以甲基叔丁基醚有机溶剂进行离子对提取,将收集的上清液用氮气吹干后用0.25 ml 1∶1甲醇和水溶液复溶,再经过0.2μm尼龙滤膜净化,采用Waters ACQUITYTM BEH C18色谱柱(50 mm×2.1 mm×1.7 mm)分离,在电喷雾负离子源(ESI-)和多反应监测模式(MRM)下进行测定.结果 在15种目标化合物中,全氟己基-2-次磷酸盐、全氟己基-全氟辛基-次膦酸盐、全氟辛基-2-次膦酸盐三种物质使用外标法定量,三个添加水平的回收率在41.01％ ～ 112.13％之间,RSD在1.80％～11.63％之间.其余的12种物质使用同位素内标法定量,两个添加水平的回收率在70.25％～127.51％之间,RSD均在1.23％ ～ 15.45％.15种待测物质的检出限在0.1～ 5.0 pg/ml之间,定量限在0.2～ 10.0 pg/ml之间.并且对10份人血清样品进行了目标化合物的检测,部分物质被检出,其中全氟-1-辛基磺酰胺、N-乙基全氟-1-辛基磺酰胺、N-甲基全氟-1-辛基磺酰胺乙酸、N-乙基全氟-1-辛基磺酰胺乙酸的浓度范围分别为＜ LOD ～0.94 pg/ml、＜LOD ～ 10.08 pg/ml、＜LOD ～6.74 pg/ml、＜LOD ～ 1.04 pg/ml.结论 本方法简单、快速,灵敏度和准确度高,满足研究全氟磺酸及全氟烷酸前体物质人体负荷水平的需要.
目的 建立超高效液相色譜-串聯三重四級桿質譜(UPLC-MS/MS)測定血清基質中15種全氟磺痠以及全氟烷痠前體物質的方法.方法 血清中的目標化閤物與四丁基銨硫痠氫鹽結閤後,以甲基叔丁基醚有機溶劑進行離子對提取,將收集的上清液用氮氣吹榦後用0.25 ml 1∶1甲醇和水溶液複溶,再經過0.2μm尼龍濾膜淨化,採用Waters ACQUITYTM BEH C18色譜柱(50 mm×2.1 mm×1.7 mm)分離,在電噴霧負離子源(ESI-)和多反應鑑測模式(MRM)下進行測定.結果 在15種目標化閤物中,全氟己基-2-次燐痠鹽、全氟己基-全氟辛基-次膦痠鹽、全氟辛基-2-次膦痠鹽三種物質使用外標法定量,三箇添加水平的迴收率在41.01％ ～ 112.13％之間,RSD在1.80％～11.63％之間.其餘的12種物質使用同位素內標法定量,兩箇添加水平的迴收率在70.25％～127.51％之間,RSD均在1.23％ ～ 15.45％.15種待測物質的檢齣限在0.1～ 5.0 pg/ml之間,定量限在0.2～ 10.0 pg/ml之間.併且對10份人血清樣品進行瞭目標化閤物的檢測,部分物質被檢齣,其中全氟-1-辛基磺酰胺、N-乙基全氟-1-辛基磺酰胺、N-甲基全氟-1-辛基磺酰胺乙痠、N-乙基全氟-1-辛基磺酰胺乙痠的濃度範圍分彆為＜ LOD ～0.94 pg/ml、＜LOD ～ 10.08 pg/ml、＜LOD ～6.74 pg/ml、＜LOD ～ 1.04 pg/ml.結論 本方法簡單、快速,靈敏度和準確度高,滿足研究全氟磺痠及全氟烷痠前體物質人體負荷水平的需要.
목적 건립초고효액상색보-천련삼중사급간질보(UPLC-MS/MS)측정혈청기질중15충전불광산이급전불완산전체물질적방법.방법 혈청중적목표화합물여사정기안류산경염결합후,이갑기숙정기미유궤용제진행리자대제취,장수집적상청액용담기취간후용0.25 ml 1∶1갑순화수용액복용,재경과0.2μm니룡려막정화,채용Waters ACQUITYTM BEH C18색보주(50 mm×2.1 mm×1.7 mm)분리,재전분무부리자원(ESI-)화다반응감측모식(MRM)하진행측정.결과 재15충목표화합물중,전불기기-2-차린산염、전불기기-전불신기-차련산염、전불신기-2-차련산염삼충물질사용외표법정량,삼개첨가수평적회수솔재41.01％ ～ 112.13％지간,RSD재1.80％～11.63％지간.기여적12충물질사용동위소내표법정량,량개첨가수평적회수솔재70.25％～127.51％지간,RSD균재1.23％ ～ 15.45％.15충대측물질적검출한재0.1～ 5.0 pg/ml지간,정량한재0.2～ 10.0 pg/ml지간.병차대10빈인혈청양품진행료목표화합물적검측,부분물질피검출,기중전불-1-신기광선알、N-을기전불-1-신기광선알、N-갑기전불-1-신기광선알을산、N-을기전불-1-신기광선알을산적농도범위분별위＜ LOD ～0.94 pg/ml、＜LOD ～ 10.08 pg/ml、＜LOD ～6.74 pg/ml、＜LOD ～ 1.04 pg/ml.결론 본방법간단、쾌속,령민도화준학도고,만족연구전불광산급전불완산전체물질인체부하수평적수요.
Objective We established a method of UPLC-MS/MS that was to detect fifteen precursors of perfluoroalkyl sulfonates (PFSA) and perfluoroalkyl carboxylates (PFCA) in serum.Methods Briefly,TBAS solution was added to sera,then the mixed solution was extracted with aliquots of MTBE.The MTBE aliquots were combined,evaporated to dryness under nitrogen,and reconsituted in 0.25 ml of methanol and water (1∶1).Then the reconstituted solution through 0.2 μm nylon syringe filter was collected.Chromatographic separation was performed using a Waters ACQUITYTM BEH 18C column (50 mm × 2.1 mm × 1.7 mm).Analyte quantitation was performed in the negative electrospray ionization mode and multiple reaction monitoring (MRM).Results Three target substances,6:6PFPi,6:8PFPi,8:8PFPi,were externally confirmed by standard addition.Rates of recovery for these three chemicals were from 41.01％ to 112.13％ in two standard levels.And the relative standard deviations (RSD) were lower than 11.63％ and higher than 1.80％.The other twelve substances were quantified with internal standard.Moreover in two standard levels,rate of recovery for these chemicals ranged from 70.25％ to 127.51％.And RSD were more than 1.23％ and less than 15.45％.And the corresponding limit of detection (LOD) and limit of quantitation (LOQ) for all target substances were 0.1-5.0 pg/ml and 0.2-10.0 pg/ml.Then we detected these target substances in ten different human serum samples.The levels of few substances were higher than LOD.And the ranges of FOSA-M,N-EtFOSA-M,N-MeFOSAA,N-EtFOSAA were respectively ＜ LOD-0.94 pg/ml,＜ LOD-10.08 pg/ml,＜ LOD-6.74 pg/ml,＜ LOD-1.04 pg/ml.Conclusion The method,with high sensitivity and accuracy,could meet the actual testing requirements.
