蜂蜜中氯霉素痕量残留测量质谱基质效应研究

Mass Spectrometry Matrix Effect Study for the Trace Analysis of Chloramphenicol Residues in Honey

有机同位素稀释质谱法(Isotope dilution mass spectrometry,IDMS)是复杂基质样品中痕量成分准确测量的潜在基准方法,但分析条件、同位素稀释试剂、基质效应(Matrix Effect,ME)等因素也会对结果产生影响。本文以枣花和荆花蜂蜜为研究样品,比较不同提取方法下蜂蜜中氯霉素痕量残留测量时的基质效应,研究基质效应对结果的影响、基质效应的补偿及消除方法。采用基质效应柱后注射定性评价方法和萃取后添加定量评价方法,考察直接稀释提取法和乙酸乙酯提取法的基质效应及其对氯霉素测量结果准确性的影响;结果表明,直接稀释提取溶液中氯霉素受到的基质抑制效应更为显著,ME在7%~10%之间,抑制了90%以上的氯霉素质谱响应,外标法校准的提取回收率仅为10.9%±1.9%;乙酸乙酯法提取溶液的ME在33%~35%之间,基体抑制相对较弱,外标法校准的提取回收率为33.7%±1.2%。采用同位素稀释质谱法进行校准,两种提取方法的回收率分别为100.4%±4.3%、100.2%±3.4%,说明基质抑制效应对测量结果的影响被有效补偿。直接稀释提取法采用IDMS校准,可准确、快速测量蜂蜜中氯霉素痕量残留。

Organic isotope dilution mass spectrometry(IDMS)is a potential reference method for the accurate measurement of trace components in complex matrix samples.However,the analytical conditions,isotope dilution reagents,matrix effects(MEs),and other factors can also affect the results.In this paper,jujube and wattle honey were used as the study samples to compare the MEs in the trace measurement of chloramphenicol residues in honey under different extraction methods,so as to investigate the influence of MEs on the results,the compensation and elimination methods of MEs.