滤过型固相萃取柱净化-超高效液相色谱-串联质谱法测定鸡蛋中15种全氟化合物的含量  

Determination of 15 Perfluorinated Compounds in Eggs by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry with Filterable Solid Phase Extraction Column Purification

作　　者：吴坤 吴玉田 赵君 周贻兵[2] WU Kun;WU Yutian;ZHAO Jun;ZHOU Yibing(School of Chemistry and Materials Science,Guizhou Education University,Guiyang 550018,China;Laboratory Center,Guizhou Center for Disease Control and Prevention,Guiyang 550004,China)

机构地区：[1]贵州师范学院化学与材料学院,贵阳550018 [2]贵州省疾病预防控制中心实验中心,贵阳550004

出　　处：《理化检验（化学分册）》2024年第1期60-66,共7页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：贵州省普通高等学校青年科技人才成长项目(黔教合KY字[2021]243)。

摘　　要：提出了滤过型固相萃取柱净化-超高效液相色谱-串联质谱法同时测定鸡蛋中全氟丁酸、全氟戊酸、全氟己酸、全氟庚酸、全氟辛酸、全氟壬酸、全氟癸酸、全氟十一酸、全氟十二酸、全氟十三酸、全氟十四酸、全氟丁烷磺酸、全氟己烷磺酸、全氟庚烷磺酸、全氟辛烷磺酸等15种全氟化合物含量的方法。鸡蛋样品(2 g)中加入0.1 mL 20.0μg·L^(-1)同位素内标混合溶液,经10 mL 80%(体积分数)乙腈溶液振荡和超声提取后,离心;分取5 mL滤液,直接过滤过型Captive EMR-Lipid柱净化,收集流出液,氮吹至近干,加入500μL甲醇复溶,经涡旋、离心处理后测定。采用Agilent Eclipse Plus C_(18)RRHD色谱柱(100 mm×2.1 mm,1.8μm)分离,以不同体积比的2 mmol·L^(-1)乙酸铵溶液和甲醇的混合溶液梯度洗脱,在电喷雾离子源负离子扫描模式下,以多反应监测模式检测,同位素内标法定量。结果表明:15种全氟化合物标准曲线的线性范围均为0.125~20.0μg·L^(-1),测定下限(10S/N)为0.05~0.16μg·kg^(-1);在0.500,4.00,16.0μg·kg^(-1)加标浓度水平下,15种目标物的回收率为78.0%~111%,测定值的相对标准偏差(n=6)为0.87%~14%。A method for the determination of 15 perfluorinated compounds,including perfluorobutyric acid,perfluoropentanoic acid,perfluorohexanoic acid,perfluoroheptanoic acid,perfluorooctanoic acid,perfluorononanoic acid,perfluorodecanoic acid,perfluoroundecanoic acid,perfluorododecanoic acid,perfluorotridecanoic acid,perfluorotetradecanoic acid,perfluorobutane sulfonate,perfluorohexane sulfonate,perfluoroheptane sulfonate and perfluorooctane sulfonate,in eggs by ultra-high performance liquid chromatography-tandem mass spectrometry with filterable solid phase extraction column purification was proposed.The 0.1 mL of 20.0μg·L^(-1)the isotope standard mixed solution was added into 2 g of egg sample,and the mixture was extracted by oscillation and ultrasonic with 10 mL of 80%(volume fraction)acetonitrile solution.After centrifugation,5 mL of the filtrate was taken and directly passed through Captive EMR-Lipid column for purification.The effluent was collected,and blown to nearly dryness by nitrogen.The residue was redissolved with 500μL of methanol,and then determined after treatment by vortex and centrifugation.The separation was performed on Agilent Eclipse Plus C_(18)RRHD column(100 mm×2.1 mm,1.8μm),and the mixed solutions composed of 2 mmol·L^(-1)ammonium acetate solution and methanol at different volume radios was used for gradient elution.Multi-reaction monitoring mode was used for detection with scanning by electrospray ion source negative ion mode,and quantification by isotope internal standard method.It was shown that the linear ranges of standard curves for 15 perfluorinated compounds were found in the same range of 0.125-20.0μg·L^(-1),with lower limits of determination(10S/N)in the range of 0.05-0.16μg·kg^(-1).The recoveries of 15 targets were in the range of 78.0%-111%at spiked concentration levels of 0.500,4.00,16.0μg·kg^(-1),and RSDs(n=6)of the determined values range from 0.87%to 14%.

关 键 词：全氟化合物 鸡蛋 超高效液相色谱-串联质谱法 Captive EMR-Lipid柱 

分 类 号：O657.63[理学—分析化学]