高效液相色谱法测定水产品中乙氧喹啉残留

Determination of ethoxyquin in aquatic products by high performance liquid chromatography

建立了高效液相色谱-荧光检测器(HPLC-FLD)检测水产品中乙氧喹啉残留量的方法。试样加入碳酸钠溶液和丙酮振荡提取后,用正己烷进行液-液萃取分配,取正己烷层浓缩近干后,再用乙腈溶解,溶解液经氧化铝固相萃取小柱净化,收集所有过滤液,氮气吹干定容后,用配有荧光检测器的高效液相色谱仪测定,外标法定量。结果表明,乙氧喹啉在0.01～10μg/mL的范围内呈良好的线性关系,相关系数为0.9997。在添加浓度为0.01、0.02、0.5、1.0和2.0mg/kg5个添加水平下,样品的平均回收率为71.2%～94.7%,相对标准偏差小于10%;方法的测定低限为0.01mg/kg。该方法操作简便、净化效果好、灵敏度高,适用于水产品中乙氧喹啉的检测。

An analytical method was developed for the determination of ethoxyquin in aquatic products by high per-formance liquid chromatography with fluorescence detector （ HPLC - FLD）. The sample was firstly extracted with sodi- um carbonate solution and acetone, and then n - hexane was used for liquid - liquid extraction. The n - hexane layer was taken for further concentration, the residue was dissolved by acetonitrile, and then cleaned -up with a neutral a- lumina solid phase extraction column. All the filtration was collected and blown to dryness by nitrogen gas. The ana- lytes were determined by HPLC -FLD and quantified by external standard method. The results showed that the cali- bration curve showed good linearity in the range from 0.01 Ixg/mL to 10 mg/kg. For the added concentration at 0.01 mg/kg, 0.02 mg/kg,0.5 mg/kg, 1.0 mg/kg and 2.0 mg/kg, the average recoveries of sample were from 71.2 % to 94.7 %. The relative standard deviations were less than 10 %. The limit of detection was 0.01 mg/kg. The results indicated that the pretreatment method was easy, effective, sensitive and suitable for the determination of ethoxyquin in aquatic products.