高效液相色谱—串联质谱法检测鸡蛋中五氯酚钠药物残留研究  

Determination of pentachlorophenol sodium residues in eggs by high performance liquid chromatography tandem mass spectrometry

作　　者：张美 朱莉莎 徐飘飘 吴双敏 梁继翔 彭大鹏[2] Zhang Mei;Zhu Lisha;Xu Piaopiao;Wu Shuangmin;Liang Jixiang;Peng Dapeng(Wuhan Industrial Control Testing Company Limited,Hubei Wuhan 430030;Huazhong Agricultural University,Hubei Wuhan 430070)

机构地区：[1]武汉工控检验检测有限公司,湖北武汉430030 [2]华中农业大学,湖北武汉430070

出　　处：《现代畜牧兽医》2023年第3期19-22,共4页Modern Journal of Animal Husbandry and Veterinary Medicine

基　　金：国家自然科学基金(31772074)。

摘　　要：研究旨在建立一种检测鸡蛋中五氯酚钠(PCP-Na)药物残留的高效液相色谱-串联质谱分析方法。pH值为6.6~6.8时,PCP-Na可全部转化为五氯酚(PCP),可通过检测PCP含量测定鸡蛋样品中PCP-Na药物残留量。采用5%氨水-乙腈超声提取2次后,用Agilent Bond Elut Plexa PAX固相萃取柱净化,洗脱液氮吹浓缩至近干,复溶过滤后采用高效液相色谱-串联质谱法检测,以5 mmol/L乙酸铵溶液与甲醇为流动相体系。结果显示,PCP-Na在0.5~20.0μg/L浓度范围内具有良好的线性关系(R^(2)>0.999),检出限为0.5μg/kg,定量限为1.0μg/kg,平均回收率为78.99%~81.92%,相对标准偏差为0.18%~0.20%。研究表明,该检测方法有效避免了样品中基质干扰,且简便、快速、准确可满足鸡蛋中PCP-Na残留限量检测。A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) method was developed for the determination of sodium pentachlorophenol(PCP-Na) residues in eggs. All PCP-Na was converted to pentachlorophenol(PCP) at pH 6.6~6.8, so PCP-Na residues in egg samples could be determined by PCP content. The samples were extracted twice with 5% ammonia-acetonitrile, cleaned up with an Agilent Bond Elut Plexa PAX solid phase extraction column, and the eluate was concentrated by nitrogen blowing to near dryness, and detected by high performance liquid chromatography-tandem mass spectrometry after re-dissolution and filtration with 5 mmol/L ammonium acetate solution and methanol as the mobile phase system. The results showed that PCP-Na showed good linearity(R^(2)>0.999) in the concentration range of 0.5~20.0 μg/L, with the detection limit of 0.5 μg/kg and the quantification limit of 1.0 μg/kg,and the average recoveries ranged from 78.99% to 81.92% with the relative standard deviations of 0.18%~0.20%. The study indicated that the method could effectively avoid matrix interference in the samples, and was simple, rapid and accurate for the detection of PCP-Na residue limit in eggs.

关 键 词：高效液相色谱-串联质谱 五氯酚钠 鸡蛋 药物残留 

分 类 号：S816[农业科学—饲料科学]