免疫亲和柱净化-液相色谱-串联质谱法同时测定猪肉中6种玉米赤霉醇类化合物残留量

Simultaneous Determination of Residues of Six Kinds of Zeranols in Pork by High Performance Liquid Chromatography-Tandem Mass Spectrometry and Cleaned up by Immunoaffinity Column

建立了猪肉中6种玉米赤霉醇类化合物残留量的免疫亲和柱净化-液相色谱-串联质谱(IAC-LC-MS/MS)分析方法。酶解后的样品用乙醚提取,提取液浓缩后用三氯甲烷溶解,NaOH溶液反萃取,经免疫亲和柱富集和净化后,采用LC-MS/MS进行测定,外标法定量。在Shimadzu Shim-pack VP-ODS C18反相柱上分离,梯度洗脱,流动相为乙腈和2 mmol/L乙酸铵溶液;质谱采集为电喷雾负离子多反应监测模式。6种目标物的线性范围为0.5～200μg/L,相关系数(R)大于0.999,定量限(LOQ)在0.05～0.63μg/kg之间;添加浓度在1.0～5.0μg/kg范围内,方法回收率为71.3%～93.7%,相对标准偏差在3.7%～9.7%之间。该方法灵敏度高、重现性好,适用于猪肉样品中痕量玉米赤霉醇类药物残留的测定。

A method was established for the determination of residues of six kinds of zeranols in pork based on immunoaffinity column（IAC） purification by high performance liquid chromatography tandem mass spectrometry（LC-MS/MS）.Enzymolyzed samples were extracted with ethyl ether,and the extract was vacuum concentrated to dryness and dissolved in trichloromethane.After re-extracted with sodium hydroxide solution and cleaned up by immunoaffinity column,the analyses were carried out on LC-MS/MS.The chromatographic separation was performed on a Shimadzu Shim-pack VP-ODS C18 column with gradient elution by using acetomitrile and 2 mmol/L ammonium acetate solution as mobile phases.Detection was carried out by electrospray negative ionization mass spectrometry in the multiple reaction monitoring（MRM） mode.The linearities（R0.999） were achieved for the 6 compounds over the range of 0.5-200 μg/L.The quantification limits of the method were 0.05-0.63 μg/kg.The recoveries of the 6 compounds were 71.3%-93.7%,and the relative standard deviations were 3.7%-9.7%.The method is sensitive,reproducible,and applicable to analysis trace residues of zeranols in pork.