为建立适用于动物源性食品中泰地罗新残留量检测的高效液相色谱-串联质谱法(HPLC-MS/MS),本研究对色谱、质谱、净化条件和定溶液等进行检测条件优化,建立了测定动物源性食品中泰地罗新残留量的检测方法,验证其线性范围、检出限,并以猪、牛、羊肉及其内脏等动物源性食品为试验样品,测定其回收率及精密度.结果表明,色谱条件以Aglient ZORBAX SB C18为色谱柱,乙腈-0.1%甲酸水为流动相;质谱条件以734.4 m/z为母离子,98.2和174.4 m/z为子离子;净化条件以HLB(150 mg,6 mL)固相萃取柱为净化柱,5 mL 50%甲醇水溶液为上样溶液,5 mL 5%氨水乙腈为洗脱溶剂;定容液为0.1%甲酸水-乙腈(v/v,9/1).该方法在5～50 μg/L范围内线性良好,线性相关系数为0.999 7,检出限为5 μg/kg,动物源性食品的泰地罗新回收率81.8%～110.6%,相对标准偏差在1.38%～7.14%.本方法准确度较高,适用于动物源食品中泰地罗新残留量检测.
Determination of Tildipirosin in animal-origin foodstuffs by HPLC-MS/MS
To establish a high performance liquid chromatography-mass spectrometry(HPLC-MS/MS)method suitable for the detection of residues of Tildipirosin in animal-origin foodstuffs.Chromatography,mass spectrometry,purification conditions and solution were optimized to establish a method for the determination of residues of Tildipirosin in animal-origin foodstuffs.The recovery and precision of animal derived food such as pig,cow,mutton and offal were measured.The results showed that The chromatographic conditions were Aglient ZORBAX SB C18 column and acetonitrile-0.1%formic acid water as mobile phase.The mass spectrum conditions were 734.4 m/z as parent ion,98.2 m/z and 174.4 m/z as daughter ion.The purification condition were HLB(150 mg,6 mL)solid phase extraction column as the purification column,5 mL 50%methanol aqueous solution was used as the sample solution,and 5 mL 5%aminoacetonitrile was used as the elution solvent.The constant volume solution was 0.1%formic acid water-acetonitrile(v/v,9/1).The linear correlation coefficient was 0.999 7,the detection limit was 5 μg/kg,the recovery rate of Tildipirosin in animal-origin foodstuffs was 81.8%-110.6%,and the relative standard deviation was 1.38%-7.14%.The method had high accuracy and was suitable for the detection of residues of Tildipirosin in animal-origin foodstuffs.
万方数据
维普
