在聚氯乙烯（PVC）塑料玩具样品（1.00 g，预先剪碎）中，加乙酸乙酯（10 mL）进行微波萃取（90℃，50 min），萃取液蒸缩至5 mL，以全氟辛烷磺酸（PFOS）分子印迹聚合物（PFOS-MIP，3 g）作为基质分散固相萃取（MSPD）的吸附剂，提取样品中的PFOS，用甲醇（5 mL）从分子印迹聚合物上洗脱PFOS，并使洗脱液与衍生化试剂10%（体积分数）四丁基氢氧化铵（TBAH）溶液（400 μL）在60℃反应60 min，生成挥发性较好的全氟辛基磺酸丁酯，加正己烷将溶液定容至1 mL，按仪器工作条件进行气相色谱-质谱法测定。对衍生化反应的时间、温度、TBAH溶液的用量等条件用响应面分析法进行了试验，确定了上述反应的最佳条件。结果表明：PFOS的质量浓度在1~200 μg·L^-1内与其对应的峰面积呈线性关系，方法的检出限（3S/N）为0.95 μg·L^-1。用标准加入法进行回收试验，测得回收率为89.6%~95.2%，测定值的相对标准偏差（n=10）为6.4%~8.3%。

The sample of PVC plastic toys (1.00 g, to be cut up previously) was extracted in a microwave extractor with ethylacetate (10 mL) for 50 min at 90℃. The extract was evaporated to 5 mL, and perfluorooctane sulfonates (PFOS) in it were extracted by MSPD extraction using PFOS-MIP (3 g) as adsorbent. PFOS adsorbed on the MIP were eluted with methanol (5 mL). The eluate was derivatized by reaction with 400 μL of TBAH solution (10%, φ) for 60 min at 60℃, to give butyl perfluorooctane sulfonate with better volatility. n-Hexane was added to the solution to make its volume to 1 mL, and used for GC-MS determination under the prescribed conditions. The time, temperature and amount of TBAH solution for the derivatization were tested and studied by applying the response surface analysis, and optimum conditions were determined. It was found that linear relationship was kept between mass concentration of PFOS in the range of 1-200 μg·L^-1 and values of respective peak area. Detection limit (3S/N) of the method was 0.95 μg·L^-1. Recovery was tested by standard addition method, giving values of recovery ranged from 89.6% to 95.2%. Values of RSDs (n=10) found were in the range of 6.4%-8.3%.