基于环境友好的样品前处理方法研究及其在兽药残留检测中的应用

The traditional sample pretreatment methods always bring about enormous quantities of toxic pollutants, which would pollute environment and injure the health of the analyst. It becomes an even more pressing task to develop environment-friendly sample pretreatment method. An organic solvent free method will be developed to extract chloramphenicol(CAP), diethylstilbestrol(DES) and zeranol(ZER) in animal foodstuffs by studying physico-chemical properties of the drugs and characters of the samples. CAP, DES and ZER will be modified and made into protein conjugate to develop anti-CAP, anti-DES and anti-ZER monoclonal antibodies (Mabs) respectively. Studying couple mechanism, selecting suitable condition, coupling these three Mabs to the solid support respectively, optimizing correlated parameters and screening green solvents, the environment-friendly immnuoaffinity chromatography-microextraction in packed syringe, immnuoaffinity chromatography-stir rod sorptive microextraction and immnuoaffinity chromatography-etched stainless steel wire microextraction sample pretreatment method will be developed. In this program, based on the demand of the foodstuff safety and environmental protection of our country, the immnuoaffinity chromatography-microextraction in packed syringe, immnuoaffinity chromatography-stir rod sorptive microextraction and immnuoaffinity chromatography-etched stainless steel wire microextraction will be used in sample pretreatment method in the residues analysis, which will be used for reference and provide basic theory for developing originality environment-friendly method in residues determination.

传统的样品前处理方法往往伴随着大量的污染产生，既危害环境又损害分析者的身体健康，迫切需要发展环境友好的样品前处理方法。通过研究相关药物（氯霉素、己烯雌酚和玉米赤霉醇）的理化性质和样品基质的特点，分别建立无有机溶剂的提取方法；通过选取相关药物（氯霉素、己烯雌酚和玉米赤霉醇）进行结构改造并设计蛋白结合物，分别制备具有簇特异性的单克隆抗体；通过研究抗体的偶联机制，选择合适的方法，分别将单克隆抗体与相关载体偶联，优化相关参数，筛选绿色溶剂，建立环境友好的免疫亲和-填充吸附剂式微萃取、免疫亲和-搅拌头吸附微萃取和免疫亲和-刻蚀不锈钢丝微萃取样品前处理方法。本项目旨在围绕国家食品安全和保护环境的需求，将免疫亲和色谱与填充吸附剂式微萃取、搅拌头吸附微萃取和刻蚀不锈钢丝微萃取结合应用于样品前处理，减少有机溶剂的用量，为探索原创性的环境友好的兽药残留检测方法提供理论基础和科学借鉴。

动物性食品中的兽药残留严重危害人类的健康，传统的样品前处理方法往往伴随着大量的污染产生，既危害环境又损害分析者的身体健康。本研究建立了环境友好的可以分离净化动物源性食品中药物残留的免疫亲和色谱-填充吸附剂式注射器微萃取、免疫亲和色谱-玻璃搅拌棒吸附微萃取和免疫亲和色谱-刻蚀不锈钢棒微萃取前处理方法，并将其与液相色谱串联质谱（LC-MS/MS）和液相色谱荧光检测法（LC-FLD）结合，建立了相关残留检测方法，为残留监控提供常规定量和确证手段，为建立新的药物残留检测方法提供借鉴。建立了免疫亲和色谱-填充吸附剂式注射器微萃取-LC-FLD测定牛奶中8种喹诺酮类药物方法；建立了免疫亲和色谱-填充吸附剂式注射器微萃取-UPLC-MS/MS测定牛奶中6种玉米赤霉醇类化合物方法；建立了可以检测牛奶中11种喹诺酮类药物的免疫亲和色谱-玻璃搅拌棒吸附微萃取-LC-FLD方法；建立了免疫亲和色谱-刻蚀不锈钢棒微萃取-UPLC-MS/MS测定环境水样中3种二苯乙烯类雌激素方法；初步建立了免疫亲和色谱-刻蚀不锈钢棒微萃取-UPLC-MS/MS测定牛奶中3种二苯乙烯类雌激素方法；建立了QuEChERS-LC-FLD检测牛肉中的阿维菌素类药物方法；建立了水提取-UPLC-MS/MS测定猪肉中氯霉素的方法。环境友好的前处理方法可以降低有机溶剂用量，减少环境污染，具有十分重要的意义。