HPLC-APCI(+)MS/MS内标法测定水产品中的3种硝基咪唑类药物残留量

Determination of three nitroimidazole residues in aquatic products by high performance liquid chromatography APCI(+)/tandem mass spectrometry with internal standard method

中文关键词: 高效液相色谱-串联质谱  大气压化学源（APCI）  内标法  甲硝唑  二甲硝唑洛硝哒唑  残留  水产品

英文关键词: High performance liquid chromatography tandem mass spectrometry  Atmospheric pressure chemical ionisation(APCI)  Internal standard methodMetronidazole  Dimetridazole  Ronidazole  ResiduesAquatic products

中文摘要:

      建立了水产品中3种硝基咪唑类残留量的HPLC-APCI(+)MS/MS测定方法。以氘代二甲硝唑(DMZ-D3)作为内标，以乙酸乙酯提取水产品中残留的硝基咪唑类药物，采用HPLC-MS/MS多反应监测(MRM)正离子模式测定，可一次对水产品中的MTZ、DMZ和RNZ进行定性和定量。该法简便快捷，适合大批量样品处理。方法简化了样品前处理过程，省去固相萃取步骤，具有操作简便和有机试剂消耗量少等优点。DMZ、MTZ和RNZ的检出低限均为0.5 μg/kg，DMZ、MTZ和RNZ的定量下限均为1.0 μg/kg。

英文摘要:

      The method for the determination of three nitroimidazole residues in aquatic products was developed by high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS). Deuterated dimetridazole (DMZ-D3) was added to the sample as internal standard before extraction. The sample was extracted with ethyl acetate. The mass spectrometer was operated in the positive ion mode using multiple reaction monitoring for qualitative and quantitative analysis of MTZ,DMZ and RNZ at the same time. The preliminary treatment included predigestion，and no solid phase extraction(SPE) procedure was adopted. The advantage of the method was simple operation，less organic chemicals consumed，and shorter operation time. The limits of detection for DMZ,MTZ and RNZ were 0.5 μg/kg. The limits of quantitation for DMZ、MTZ and RNZ were 1.0 μg/kg.