中文摘要：

本研究采用HPLC-MS/MS联用技术,建立了分析人血清样品中全氟辛酸（PFOA）、全氟辛烷磺酸（PFOS）及7种PFOS前体物的方法.以Fluoro Sep RP Octyl反相柱为色谱分离柱,甲醇和醋酸铵为梯度洗脱淋洗液,内标校正法进行定量分析.比较了3种不同萃取方法对目标全氟化合物的萃取性能,结果表明乙腈/乙酸乙酯（体积比60∶40）混合溶剂的萃取效率最高.提取液进质谱分析前,预先过石墨烯柱进一步净化以减轻基质效应和延长色谱柱寿命.9种目标全氟烷基化合物在0.50—50μg·L^（-1）浓度范围内线性相关系数r均大于0.995,检出限为0.013—0.083μg·L^（-1）,定量限为0.043—0.28μg·L^（-1）.在添加浓度为0.50、1.0、5.0μg·L^（-1）水平下,9种全氟烷基化合物的加标回收率为81.7%—108%,相对标准偏差均小于12%.本方法稳定性好、准确度高、且可同时分析不同种类的PFOS前体以及PFOA和PFOS的异构体,适用于实际人体血清样品的定量分析检测.对10份中国人体血清样品的分析结果表明,PFOA和PFOS的浓度分别为0.60—5.1μg·L^（-1）和1.2—63μg·L^（-1）,总支链PFOA的含量比例为3.0%—12%,总支链PFOS的含量比例为32%—69%.N-Me FOSAA在一个血清样品中被检出,其浓度为0.92μg·L^（-1）.2个血清样品中含有全氟辛烷磺酰胺（FOSA）,其浓度为0.12μg·L^（-1）和0.17μg·L^（-1）.

英文摘要：

A sensitive method was developed for the quantification and quantitation of perfluorooctanoate（ PFOA）,perfluorooctane sulfonate（ PFOS）,and seven PFOS precursors in human serum samples. The target compounds were separated on a Fluoro Sep RP Octyl column using methanol and ammonium acetate solution as mobile phases by gradient elution. Three differentextraction methods were compared for the extraction efficiency of target perfluorochemicals in human serum samples,and acetonitrile / ethyl acetate（ volume ratio 60 ∶ 40） was selected as the best extraction solvent. Further purification using Envi-Carb solid phase extraction columns was introduced to reduce the matrix effect and protect the chromatographic column. The calibration curve was linear in the range of 0.50—50 μg·L~（-1）with a correlation coefficient（ r） larger than 0.995. The limits of detection（ LOD） of analytes were in the range of 0.013—0.083 μg·L~（-1）,while the limits of quantitation（ LOQ） were in the range of 0. 043—0. 28 μg·L~（-1）. At spiking concentrations of 0. 50,1.0,and 5. 0 μg·L~（-1）,the recoveries of nine analytes were in the range of 81. 7%—108% with relative standard deviations 12%. PFOA,PFOS（ including branched isomers） and a variety of PFOS precursors could be well separated and quantitated with good stability and high accuracy. The target compounds in 11 human serum samples from China were analyzed with the concentrations of0.60—5.1 μg·L~（-1）and 1. 2—63 μg·L~（-1）for PFOA and PFOS,respectively. The proportion of total branched PFOA and PFOS was 3. 0%—12% and 32%—69%,respectively. N-Me FOSAA was detected in a serum sample and its concentration was 0. 92 μg·L~（-1）. Two serum samples contained FOSA with the concentration of 0.12 μg·L~（-1）and 0.17 μg·L~（-1）.