鱼塘水样采用全自动在线顶空固相微萃取进行萃取：萃取温度为75℃；萃取时间为60 min；氯化钠加入量为0.3 kg·L^-1；样品体积为2.0 mL。采用气相色谱-串联质谱法测定水样中硫丹（α-硫丹、β-硫丹）和硫丹硫酸酯的含量，在气相色谱分离中采用DB-5 ms毛细管色谱柱，在串联质谱分析中采用多反应监测模式。α-硫丹、β-硫丹和硫丹硫酸酯的质量浓度在一定范围内与其对应的峰面积呈线性关系，检出限（3S/N）为0.001~0.015 μg·L^-1，测定下限（10S/N）为0.003~0.050 μg·L^-1。以空白水样为基体进行加标回收试验，所得回收率为83.6%~117%，测定值的日内相对标准偏差（n=6）为2.2%~18%，日间相对标准偏差（n=3）为4.2%~18%。

The fishpond water samples were extracted with fully automatic online HS-SPME. Temperature of extraction was 75℃, time of extraction was 60 min, adding amount of sodium chloride was 0.3 kg·L^-1 and sample volume was 2.0 mL. GC-MS/MS was applied to the determination of endosulfan(α-endosulfan and β-endosulfan) and endosulfan sulfate in water samples. The DB-5 ms capillary chromatographic column was used for GC separation and the multiple reaction monitoring mode was adopted in MS/MS determination. Linear relationships between values of peak area and mass concentration of α-endosulfan, β-endosulfan, and endosulfan sulfate were kept in definite ranges, with detection limits (3S/N) in the range of 0.001-0.015 μg·L^-1 and lower limits of determination (10S/N) in the range of 0.003-0.050 μg·L^-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 83.6%-117%, with intra-day RSDs (n=6) of determined values in the range of 2.2%-18% and inter-day RSDs (n=3) in the range of 4.2%-18%.