水产品中孔雀石绿和结晶紫残留的拉曼光谱法快速检测

Rapid Determination of Malachite Green and Crystal Violet Residues in Aquatic Products by Raman Spectroscopy

摘要:

为实现水产品中孔雀石绿以及结晶紫残留的快速检测，建立了一种水产品中孔雀石绿以及结晶紫残留的表面增强拉曼光谱（SERS）快速检测方法。该方法通过乙腈提取、石油醚净化、硼氢化钾还原以及二氯二氰苯醌（DDQ）氧化等四步获取提取液，并通过单因素实验，确定了胶体金、提取液以及促凝剂的加入量。经研究，孔雀石绿拉曼特征位移为795、39、1215、1610 cm-1，结晶紫拉曼特征位移为795、939、1610 cm-1，根据其拉曼光谱特征峰及其强度，对孔雀石绿和结晶紫进行定性快速测定。结合检出概率模型（POD），确定出孔雀石绿及结晶紫的虾、蟹类检出限为1.00 μg/kg，鱼、贝类检出限为0.50 μg/kg，灵敏性≥95%，特异性≥95%，假阴性≤5%，假阳性≤5%符合了快速检测定性的要求。该方法操作简单、快速准确，从样品前处理到结果显示仅需40 min，可用于水产品中的孔雀石绿和结晶紫的现场快速检测。

Abstract:

In order to realize the rapid detection of malachite green and crystal violet residues in aquatic products, a rapid surface enhanced Raman spectroscopy method (SERS) for malachite green and crystal violet residues in aquatic products was established. By means of acetonitrile extraction, petroleum ether purification, potassium borohydride reduction and DDQ oxidation, the amount of colloidal gold, extract and coagulant was determined. The Raman characteristic displacement of malachite green was 795, 939, 1215, 1610 cm-1. The Raman displacement of crystal violet was 795, 939, 1610 cm-1. According to its Raman spectrum characteristic peak and its intensity, the malachite green and crystal violet were determined qualitatively and rapidly. Combined with the detection probability model (POD), the detection limit of malachite green and crystal violet shrimp and crab was determined to be 1.00 μg/kg, the detection limit of fish and shellfish is 0.50 μg/kg, sensitivity ≥95%, specific ≥95%, false negative ≤5%, false positive ≤5%, which meets the qualitative requirements of rapid testing. The method is simple, rapid and accurate. It only takes 40 minutes from sample pretreatment to result display. It can be used for the on-site rapid detection of malachite green and crystal violet in aquatic products.