高效液相色谱-三重四极杆质谱法测定猪饲料、养殖用水中五氯酚的残留

Determination of Pentachlorophenol Residues in Swine Formula Feed and Farm Water Using High Performance Liquid Chromatography-triple Quadrupole Mass Spectrometry

【目的】本试验旨在建立一种测定猪饲料、饲料添加剂、水等养殖环节投入品中五氯酚残留的高效液相色谱-三重四极杆质谱方法。【方法】待测样品经碱性甲醇水溶液提取,使用阴离子固相萃取柱富集净化,经氮吹浓缩后用2%甲酸甲醇复溶,以5 mmol/L乙酸铵溶液-甲醇为流动相,经Poroshell 120 EC-C18(3 mm×100 mm,2.7μm)色谱柱分离;负离子模式下,采用多反应监测模式(multiple reaction monitoring,MRM)进行检测;使用基质匹配外标法测定五氯酚的含量,并对所建方法的线性关系、检测限(limit of detection,LOD)、定量限(limit of quantitation,LOQ)、回收率、准确度、精密度、基质效应等指标进行考察。【结果】猪饲料和饲料添加剂中五氯酚的检测限和定量限分别为0.1和0.5μg/kg,养殖用水中五氯酚的检测限和定量限分别为5和12.5 ng/L;饲料和饲料添加剂中五氯酚定量范围为0.5~20μg/kg,养殖用水中五氯酚定量范围为12.5~500 ng/L,方法线性关系良好,相关系数(R 2)均>0.999。该方法在饲料和饲料添加剂以及养殖用水中的平均加标回收率为69.8%~119.5%,相对标准偏差(relative standard deviation,RSD)为1.62%~9.86%,基质效应(matrix effect,ME)为0.62~1.29。【结论】本试验所建方法简便、快捷、灵敏度高、重复性好,适用于猪配合饲料等养殖投入品中五氯酚的测定,可为养殖环节投入品中五氯酚污染筛查提供准确高效的技术手段,从源头保障动物源性产品安全。

【Objective】A high performance liquid chromatography-triple quadrupole mass spectrometry(HPLC-MS/MS)method was developed for the determination of pentachlorophenol(PCP)in swine feed,feed additives and water.【Method】The samples were extracted with aqueous alkaline methanolic solution,enriched and cleaned up using an anionic solid phase extraction column,reconstituted with 2%formate methanol after nitrogen drying.With 5 mmol/L ammonium acetate solution-methanol as mobile phase,Poroshell 120 EC-C18(3 mm×100 mm,2.7μm)column was used to separate PCP.Under the negative ionization,multiple reaction monitoring mode(MRM)was used to determine the content of PCP.Matrix-matched external quantification method was utilized to quantitate PCP.Linear relationship,limits of detection(LOD),limits of quantification(LOQ),recovery,accuracy,precision,matrix effect and other indicators of the established method were investigated.【Result】The LOD and LOQ were 0.1 and 0.5μg/kg in livestock feed,feed ingredients and feed additives,while 5 and 12.5 ng/L in farm water,respectively.The linear range of PCP in livestock feed,feed ingredients and feed additives was from 0.5 to 20μg/kg,and the linear range of farm water was from 12.5 to 500 ng/L.The linear coefficient(R 2)was more than 0.999,showing the good linearity.In addition,the recoveries ranged from 69.8%to 119.5%and the relative standard deviation(RSD)were from 1.62%to 9.86%.The matrix effect(ME)was 0.62-1.29.【Conclusion】The method established in this study with high sensitivity,high accuracy and good robustness was suitable for the screening of PCP in swine formula feed and other farming inputs to ensure the quality and safety of meat products.