高效液相色谱-串联质谱联用法测定禽肉中二氯二甲基吡啶酚

Determination of dichorodimethyl pyridol in poultry by high performance liquid chromatography-tandem mass spectrometry

目的：研究检测食品中兽药二氯二甲吡啶酚的高效液相色谱-串联质谱联用测定方法,用于各种禽肉中二氯二甲基吡啶酚的测定。方法：用甲醇提取肉类食品中二氯二甲基吡啶酚,经氮气吹扫浓缩,过0.45μm微孔滤膜后,直接进HPLC/MS/MS测定。以甲醇＋水作流动相梯度洗脱,采用C18色谱柱分离;质谱采用电喷雾电离源阳离子模式,多反应监测检测,外标法定量。以m/z 192.0为母离子,选择m/z 87.0子离子作为定量离子,m/z 101.0子离子作为二氯二甲基吡啶酚辅助定性离子。结果：二氯二甲基吡啶酚在2～100 ng/ml浓度范围内线性良好,相关系数r=0.9997;方法检出限为0.04μg/kg,回收率在93.9%～103.5%之间,精密度为2.00%（低浓度）和1.29%（高浓度）。结论：建立的方法测定食品中二氯二甲基吡啶酚满足痕量分析要求,并具有操作简单、干扰少、快速、准确可靠等特点,可用于我国禽肉中二氯二甲基吡啶酚状况调查。

Objective：To develop a method for determination of dichorodimethyl pyridol in poultry by high performance liquid chromatography-Tandem Mass Spectrometry（HPLC/MS/MS）.Methods：The dichorodimethyl pyridol in poultry was extracted by methanol,and concentrated by Nitrogen.After filtration,and the extract was directly injected into the HPLC-MS/MS system.The HPLC separation was made on a C18 column by applying a gradient composed of water and methanol.Analyte identification and quantification were performed using multiple reaction monitoring（MRM） with one precursor ion（m/z 192.0）and two product ions（m/z 87.0 and m/z 101.0）as identifiers and electrospray ionization in positive mode.Results：The linear range of determination of dichorodimethyl pyridol was 2～100 ng/ml（r=0.9997）.The detection limit of the method was 0.04 μg/kg.The recoveries of 93.9%～103.5%,RSD of 2.00%（low concentration） and 1.29%（high concentration） were obtained.Conclusion：The method of determination of dichorodimethyl pyridol in poultry by HPLC-MS/MS is of low disturbance,easy to operate and accurate.It can be used in research of the dichorodimethyl pyridol in poultry.