全自动固相萃取-液相色谱串联质谱法测定动物源性食品中53种常见兽药残留

Determination of 53 kinds of common veterinary drug residues in animal-derived foods by automatic solid phase extraction-liquid chromatography-tandem mass spectrometry

中文关键词:  兽药残留  全自动固相萃取  液相色谱串联质谱法  动物源性食品

英文关键词:veterinary residues  automatic solid phase extraction  liquid chromatography-tandem mass spectrometry  animal-derived foods

中文摘要:

      目的 建立全自动固相萃取-液相色谱串联质谱法同时检测6类53种常见兽药残留检测的分析方法。方法 运用全自动固相萃取仪, 选取HLB、ENV、MCX等22种固相萃取小柱, 在反相萃取、离子萃取和正相萃取3种萃取机制下, 通过混合标准溶液考察各种小柱的吸附能力、净化能力和洗脱能力, 以选择合适的小柱和萃取程序, 结合液相色谱串联质谱法检测6类53种常见兽药的残留量。结果 在反相萃取机制下, ENV固相萃取小柱符合检测要求, 淋洗液为10%甲醇水, 洗脱液为甲醇、乙腈和乙酸乙酯分步洗脱。6类53种兽药检出限为0.20~5.0 μg/kg, 加标回收率为65%~118%, 相对标准偏差为1.1%~17.5%。结论 该方法具有前处理简单、检测结果准确、节能环保等特点, 适用于兽药残留检测的分析。

英文摘要:

      Objective To establish a method for simultaneous determination of 6 categories 53 kinds of common veterinary drug residues by automatic solid phase extraction-liquid chromatography-tandem mass spectrometry. Methods Automatic solid phase extraction instrument was used, and 22 kinds of solid-phase extraction columns, such as HLB, ENV and MCX, were selected, and the adsorption capacity, purification capacity and elution capacity of each column were investigated by mixing standard solution under 3 extraction mechanisms of reverse phase extraction, ion extraction and forward phase extraction, so as to select the appropriate column and extraction procedure. Combined with liquid chromatography-tandem mass spectrometry, the residues of 6 categories 53 kinds of common veterinary drugs were determined. Results Under the reversed-phase extraction mechanism, the ENV solid phase extraction cartridge met the testing requirements. The rinse was 10% methanol water, and the eluent was mixed by methanol, acetonitrile and ethyl acetate and eluted by step. The limits of detection for 53 veterinary drugs were 0.20?5.0 μg/kg, the recoveries were 65%?118% and the relative standard deviations were 1.1%?17.5%. Conclusion This method has the characteristics of simple pretreatment, accurate detection results, energy saving and environmental protection. It is suitable for the analysis of veterinary drug residue detection.