原位电离质谱快速筛查猪肉中10种磺胺

Rapid Screening of 10 Sulfonamides in Pork by Direct Analysis in in-situ Ionization Mass Spectrometry

该研究建立原位电离质谱实时快速直接分析猪肉中10种磺胺的方法,并通过基质效应、检出限和标准曲线线性相关性进行方法学评价。猪肉经粉碎后,乙腈提取并净化,采用原位电离源离子化,三重四极杆质谱直接分析,多反应监测模式检测,外标法定量。结果表明,猪肉经提取后不净化、分散固相萃取净化、固相萃取柱净化后目标化合物离子化效率分别为纯溶剂体系的0.74%、10.97%和15.58%;净化效果为固相萃取柱>净化包>不净化基质提取液;3种净化方法磺胺检出限均可达到10μg/kg;10种磺胺在10~100μg/L范围内,线性相关系数R2平均值分别为0.642、0.782和0.962。该方法具有较好的灵敏度和准确性,可广泛应用于猪肉样品中磺胺类药物的快速筛查和准确检测。

This study established an in-situ ionization mass spectrometry(RTMS)method for the real-time rapid direct analysis of 10 sulfonamides in pork,and evaluated the methodology through matrix effects,detection limits,and linear correlation of standard curves.Pork samples were ground,extracted,purified with acetonitrile,ionized using an in-situ ionization source,and directly analyzed by triple quadrupole mass spectrometry using multiple reaction monitoring mode for detection.Quantification was done using an external standard method.The results showed that the ionization efficiencies of the target compounds in pork samples,after extraction without purification,dispersed solid-phase extraction purification,and solid-phase extraction column purification,were 0.74%,10.97%,and 15.58%of the pure solvent system,respectively.The purification effect was found in the sequence of solid-phase extraction column>purification package>unpurified matrix extract.The detection limits of the three purification methods for sulfonamides could all reach 10μg/kg.The average linear correlation coefficients(R2)for the 10 sulfonamides in the range of 10 to 100μg/L were 0.642,0.782,and 0.962,respectively.This method demonstrated good sensitivity and accuracy,and could be widely applied for the rapid screening and accurate detection of sulfonamides in pork samples.