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FluoroSep 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0.50-50 μg·L-1浓度范围内线性相关系数r均大于0.995,检出限为0.013-0.083 μg·L-1,定量限为0.043-0.28 μg·L-1.在添加浓度为0.50、1.0、5.0.μg· 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0.60-5.1 μg· L-1和1.2-63 μg·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-MeFOSAA在—个血清样品中被检出,其浓度为0.92 μg·L-1.2个血清样品中含有全氟辛烷磺酰胺(FOSA),其浓度为0.12 μg·L-1和0.17 μg·L-1.
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