鸡蛋中抗病毒类药物残留量快速检测方法研究.docxVIP

PAGE 14 鸡蛋中抗病毒类药物残留量快速检测方法研究 摘 要 实验通过对鸡蛋的主要成分和抗病毒药物的结构性质进行探讨，在其他基质试验经验中，得出较为快速合理的提取和净化步骤，结合液相色谱-串联质谱（LC-MS/MS）仪器分析，在液相色谱柱的筛选、梯度洗脱溶液及顺序参数、质谱条件等进行优化，对鸡蛋中残留的金刚烷胺、金刚乙胺进行内标法定量分析检测，以达到快速的检测技术。研究确定提取方法为：在5g鸡蛋样品中，加入三氯乙酸-乙腈（9：1）混合提取液15mL，超声10min，漩涡3min，高速离心机恒温20℃下10000r/min离心5min。净化步骤为：活化过的PCX小柱中依次加入净化液2%甲酸5mL、1%甲酸乙腈3mL，真空抽干PCX小柱，用4mL氨水-乙酸铵-甲醇混合溶液进行洗脱，氮气浓缩仪50℃吹干，加入1mL溶解液0.1%甲酸甲醇与水，涡旋混合30s后过0.22μm膜。 实验检测结果表明： 在1，2，5，10μg/kg加标梯度下，两种抗病毒药物的平均回收率在80%以上，金刚烷胺的回收率高达85%，RSD为0.118~0.187；金刚乙胺的回收率为81%~98%， RSD为0.038~0.134。两种抗病毒药物的标准曲线在0~20μg/kg中呈良好线性关系，R2≥0.999。 关键词：液相色谱-串联质谱法；金刚烷胺；金刚乙胺；鸡蛋 Study on rapid detection method of antiviral drug residues in eggs Abstract In the experiment, the main components of eggs and the structural properties of antiviral drugs were discussed. In other matrix test experience, a more rapid and reasonable extraction and purification step was obtained. In combination with liquid chromatography-tandem mass spectrometry (LC-MS/MS) instrument analysis, the selection of liquid chromatography column, gradient elution solution and sequence parameters, mass spectrometry conditions, etc. were optimized to determine the residual gold in eggs.Amantadine and amantadine were quantitatively analyzed and detected by internal standard method to achieve rapid detection technology.The extraction method was determined as follows: adding 15 mL of trichloroacetic acid-acetonitrile (9:1) mixed extract to 5 g egg sample, ultrasonication for 10 min, whirlpool for 3 min, and centrifugation for 5 min at 10,000 r/min in a high-speed centrifuge at 20 C.The purification steps are as follows: 5 mL of 2% formic acid and 3 mL of 1% acetonitrile formic acid are sequentially added into the activated PCX column, the PCX column is vacuum-dried, eluted with 4 mL ammonia-ammonium acetate-methanol mixed solution, dried at 50 C by a nitrogen concentrator, 0.1% formic acid-methanol and water are added into the 1 mL solution, and mixed by vortex for 30 s and then passed through 0.22_m membrane