动物源食品中6种甲状腺抑制剂残留的超高效液相色谱-串联质谱法检测

Determination of Six Thyreostats in Animal Derived Food by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了动物源食品中2-硫脲嘧啶、6-甲基-2-硫脲嘧啶、6-丙基-2-硫脲嘧啶、6-苯基-2-硫脲嘧啶、2-巯基-1-甲基咪唑和2-巯基苯并咪唑6种甲状腺抑制剂残留检测的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。以BEHC18柱(50mm×2.1mm,1.7μm)为色谱柱,乙腈(含0.1%甲酸)-0.1%甲酸水溶液为流动相,梯度洗脱;柱温为30℃,流速为0.3mL/min,进样量为10μL。质谱条件为:电喷雾离子源(ESI+),多反应监测(MRM)模式。结果表明:6种药物在5～500μg/L质量浓度范围内呈良好的线性关系,相关系数r2均大于0.996;方法检出限为2μg/kg,定量下限为5μg/kg;在10、25、100μg/kg3个添加水平下,方法的平均回收率为60%～107%,批内、批间RSD均小于16%。

An ultra high performance liquid chromatography-tandem mass spectrometric（UPLC-MS/MS）method was established for the determination of six thyreostats including 2-thiouracil,6-methyl-2-thiouracil,6-propyl-2-thiouracil,6-phenyl-2-thiouracil,2-mercapto-1-methylimidazole and 2-mercaptobenzimidazole in animal derived food.The separation of target compounds was performed on a BEH C18 column（50 mm×2.1 mm,1.7 μm）with mobile phase of acetonitrile containing 0.1% formic acid-0.1% formic acid at column temperature of 30 ℃.The flow rate was set at 0.3 mL/min and the injection volume was 10 μL.The detection for target compounds was carried out by MS under ESI＋ and MRM mode.The calibration curves of six thyreostats were linear in the concentrations of 5-500 μg/L with correlation coefficients（r2）larger than 0.996.The limits of detection of the method for six thyreostats were all 2 μg/kg,and the limits of quantitation were 5 μg/kg.The average recoveries from spiked meat at three concentrations levels of 10,25 and 100 μg/kg ranged from 60% to 107%,and the intra-and inter-RSDs were less than 16%.