鸡组织中磺胺对甲氧嘧啶和二甲氧苄啶残留的HPLC-MS/MS测定

建立了同时测定鸡组织中残留的磺胺对甲氧嘧啶(SMD)和二甲氧苄啶(DVD)了的高效液相色谱-串联质谱法(HPLC-MS/MS)。样品经乙腈提取,取部分提取液用正己烷脱脂后于氮气吹干,残渣用流动相溶解并定容后上机检测,外标法定量。采用C18色谱柱,流动相为乙腈和1mL/L甲酸水溶液。选择1个母离子和2个子离子进行反应监测,对磺胺对甲氧嘧啶和二甲氧苄啶残留进行定性,选择信号最强的子离子进行定量。结果显示,SMD和DVD分别在1ng/mL~200ng/mL和0.5ng/mL~100ng/mL范围内呈良好线性关系,相关系数R20.992。通过空白样品添加回收试验,所有基质中SMD和DVD的定量限分别为10μg/kg和5μg/kg,SMD和DVD分别在50、100、200μg/kg和25、50、100μg/kg 3个添加水平下的回收率为71.7%~115.0%,相对标准偏差为1.8%~13.2%,该方法定量限低,灵敏度高,重现性好,符合相关研究的要求。

Simultaneous Determination of Sulfametoxydiazine and Diaveridine Residues in Chicken Tissues by High Performance Liquid Chromatographic Tandem Mass Spectrometry

A high performance liquid chromatographic tandem mass spectrometry (LC-MS/MS)method was presented for simultaneous determination of sulfametoxydiazine and diaveridine residues in chicken. The samples were extracted with acetonitrile,then part of the extracts were cleaned up by n-hexane,fol-lowed by blowing to dryness under nitrogen gas stream,reconstitution with mobile phase before the analy-sis on HPLC-MS/MS using external standard method.The separation of analytes was performed on C18 analytical chromatographic column with a gradient elution using acetonitrile (A)and 1 mL/L formic acid (B)solution as mobile phase.The analysis of sulfametoxydiazine and diaveridine was performed under se-lective reaction monitoring(SRM)mode by selecting one parent ion and two daughter ions as qualitative i-ons,and the most abundant daughter ion as a quantitative ion.The calibration curves of SMD and DVD were linear in the concentration range of 1 ng/mL-200 ng/mL and 0.5 ng/mL-100 ng/mL respectively, with correlation coefficients more than 0.992.The quantitative limits of the method for SMD and DVD were 10 μg/kg and 5 μg/kg respectively for all matrices,and the recoveries were in the range of 71.7%-1 15.0%with RSDs of 1.8%-13.2% while blank samples were spiked with sulfametoxydiazine and diaveridine at 50, 100,200 μg/kg and 25,50,100 μg/kg,respectively.This analytical method meets the requirements for as-says.