SPE/GC-MS测定3种水产品中的喹哪啶残留

Determination of Quinalidine Anesthetic Residues in Aquatic Products by Gas Chromatography-mass Spectrometry

建立固相萃取/气相色谱-质谱法(SPE/GC-MS)测定水产品中喹哪啶麻醉剂残留的分析方法。样品用乙腈超声提取,旋转蒸发浓缩,硅胶固相萃取柱净化, DB-17MS (30 m×0.25 mm×0.25μm)色谱柱分离, GC-MS测定,外标法定量。喹哪啶麻醉剂在10~500μg/L质量浓度范围内线性关系较好,相关系数(R2)为0.999 5,方法检出限(S/N≥3)为5μg/kg,方法定量限(S/N≥10)为20μg/kg。在水产品空白样品(南美白对虾、石斑鱼和鳜鱼)中分别添加20, 40和200μg/kg这3个浓度水平的喹哪啶标准溶液,平均回收率为80.0%~98.2%;相对标准偏差(SRSD)为3.3%~11.5%。该方法可操作性强,结果准确可靠,适合用于水产品中喹哪啶麻醉剂残留分析。

A method of solid phase extraction/gas chromatography-mass spectrometry(SPE/GC-MS) was developed for the determination of quinalidine anesthetics in aquatic products.The samples were ultrasonically extracted with acetonitrile,concentrated by rotary evaporator,purified by a silica solid phase extraction column,separated on a DB-17 MS(30 m×0.25 mm×0.25 μm) column,analyzed by GC-MS and calibrated by external standard method.There was a good linear relationship of quinalidine in the concentration range of 10-500 μg/L with correlation coefficients(R2) 0.999 5.The limits of detection(S/N≥3) and limits of quantitation(S/N≥10) were 5 μg/kg and 20 μg/kg,respectively.The average recoveries for blank aquatic products(Penaeus vannamei,Epinephelus and Siniperca chuatsi) were 80.0%-98.2% at different spiked levels 20,40 and 200 μg/kg,with relative standard deviations(SRSD) of 3.3%-11.5%.The method was operable,simple,accurate and reliable,and could be used for the analysis of quinalidine anesthetic residues in aquatic products.