分散固相萃取-气相色谱法同时测定水产品中六种丁香酚类麻醉剂的残留量

Determination of six clove phenol drug residues in aquatic products by gas chromatography with dispersive solid-phase extraction

建立了同时检测水产品中六种丁香酚类麻醉剂残留量的分散固相萃取-气相色谱检测方法。样品经丙酮进行提取,旋转蒸发浓缩后定容,采用分散固相萃取（DSPE）净化,用气相色谱仪进行测定,外标法定量。六种丁香酚类化合物在0.05~10.0μg/m L的浓度范围内线性关系良好,相关系数R2为0.9995~0.9999。又分别在罗非鱼、南美白对虾、鳗鲡以及梭子蟹肌肉样品中添加0.1~1.0mg/kg的混合标准溶液,测定平均回收率在80.3%~103.2%范围内,相对标准偏差在0.7%~5.4%之间。方法的定量限（LOQ）,六种丁香酚类化合物（丁香酚、甲基丁香酚、异丁香酚、甲基异丁香酚、乙酸丁香酚酯、乙酰基异丁香酚）均为0.1mg/kg。

A dispersive solid-phase extraction-gas chromatography（GC） method had been developed for the detection of six kinds of eugenol drug residues in aquatic products at the same time. Sample was ultrasonic extracted by acetone,constant volume after rotary evaporation concentration,using dispersive solid-phase extraction（DSPE） purification,determined by gas chromatograph. External standard calibration was adopted in the determination. Six kinds of eugenol type of anesthetic showed good linearity in the concentrations range of0.05~10.0μg/m L for the standard solutions carves,and all of the correlation coefficents（R2） were in 0.9995~0.9999. At the spiked levels of 0.1~1.0mg/kg in tilapia,south America white shrimp,eel,swimming crab muscle,the average recoveries were 80.3% ~103.2%. The relative standard deviations were 0.7% ~5.4%. The limits of quantificationg（LOQ）,all of the six kinds of eugenol drug residues（Eugenol,Methyl eugenol,Iso-eugenol,Methyl iso-eugenol,Eugenol acetate,Acetyl iso-eugenol）were 0.1mg/kg.