鱼、贝类等水产品中全氟化合物分析方法的研究

Determination of 9 Perfluorinated Compounds in Aquatic Products:Fish and Shellfish

以高效液相色谱-串联质谱联用（HPLC-MS／MS）方法测定了鱼和贝类常见水产品样品中的9种全氟化合物。鱼和贝类样品前处理采用碱消解后固相萃取的方法，并选取WAX（Oasis，Waters）作为固相萃取柱，洗提液经N2浓缩定容后用HPLC-MS／MS检测。方法对标准的回收率为97．6％～120．8％，并且对实际样品也得到了很好的回收效果；除贝类样品中PFDoDA和PFTA回收率较低外，对鱼肉和贝类样品的加标回收实验都取得了较为满意的结果。目标物的分离采用Acclaim 120 C18反相柱（150mm×4．6mm，5μm），以CH3OH和50mmol／L NH4Ac为淋洗液进行二元梯度淋洗，10min内即可完成对全氟己烷磺酸（PFHxS）、全氟辛烷磺酸（PFOS）和7种全氟羧酸（C7～C12，C14）的分析，方法对样品中9种分析物的检出限可达到0．16～2．0ng／g（10μL进样）。

A method has been established to measure 9 perfluorinated compounds （PFCs）, including 2 perfluorinated sulfonates and 7 carboxylic acids （C7-C12, C14）, in aquatic products（fish and shellfish）. PFCs in fish and shellfish were extracted with a modified NaOH digestion WAX method, and the final eluate was reduced to 1 mL with nitrogen before injection. Under the optimal conditions, PFCs standards were recovered well through the whole pretreatment procedure with recoveries of 97.6% - 120.8%. When applied to fish and shellfish samples, PFCs were also well recovered, except perfluorododecanoic acid（PFDoDA） and perfluoro- tetradexanoic acid （PFTA） for shellfish. With the use of high performance liquid chromatography/electrospray tandem mass spectrometry, 9 analysts were separated on Acclaim 120 C18 reversed-phase column（ 150 mm×4.6 mm, 5μm） in 10 min using CH3OH and 50 mmol/L NH4Ac gradient elution, and a detection limit of 0.16-2.0 ng/g for real samples analysis can be achieved.