紫外/荧光检测快速测定水产品中孔雀石绿、结晶紫及其代谢物

Rapid determination of malachite,crystal violet and their metabolites in aquatic products by HPLC with ultraviolet and fluorescent detection

目的：建立水产品中孔雀石绿、结晶紫及其代谢物的紫外、荧光检测器串联检测方法。方法：样品经Mcllvaines缓冲液（pH3.0）＋乙腈混合溶液（1＋2）提取,MCX柱净化,synergy C18色谱柱（250×4.6 mm,5μm）洗脱分离,紫外、荧光检测器串联检测,外标法定量。结果：0-100μg/L范围内线性关系良好,相关系数r〉0.999,检测限0.052-1.2μg/kg,平均回收率均大于70%,相对标准偏差均小于10%。结论：方法便捷、实用,适合水产品中孔雀石绿、结晶紫及其代谢物的同时检测。

Objective：To develop a method for determination of malachite green,crystal and their metabolites in aquatic products by high performance liquid chromatography with ultraviolet and fluorescent detection.Methods： The analytes were extracted with Mcllvaines buffer（pH3.0）＋acetonitrile（1＋2） and purified by MCX solid-phase extraction cartridges.The separation was carried out on a synergy C18 column（250×4.6 mm,5 μm） with pH4.5,100 mmol/L ammonium acetate＋acetonitrile（20＋80） as mobile phase.The quantification was accomplished by external standard method.Results： The calibration curves showed good linearity for 4 analytes with detection limits of 0.052~1.2 μg/kg.The spiked recoveries in aquatic products samples ranged from 71%~93% with RSDs less than 10%.Conclusion： The method was simple,practical,and suitable for the determination of malachite green,crystal and their metabolites in aquatic products.