液相色谱-串联质谱测定鸡蛋中氯霉素残留及北京地区膳食暴露风险评估

Determination of chloramphenicol in eggs by ultra-high performance liquid chromatography-tandem mass spectrometry and dietary exposure risk assessment of chloramphenicol for Beijing

【目的】建立并优化鸡蛋中氯霉素残留的固相萃取-超高效液相色谱-串联质谱检测方法,在此基础上分析北京地区鸡蛋产品中氯霉素残留量,评估北京地区居民膳食暴露风险.【方法】采用C_(18)色谱柱进行分离,以0.1%甲酸水-0.1%甲酸甲醇溶液为流动相,梯度洗脱,在电喷雾ESI离子源负离子模式下,采用质谱多反应监测(MRM)模式进行定性分析,以内标法进行定量分析.【结果】该方法检出限(LOD)和定量限(LOQ)分别为0.008μg/kg和0.02μg/kg.在0.1~5μg/L范围内,氯霉素的质量浓度和峰面积呈现出良好的线性关系,其相关系数为0.9995;北京地区不同年龄人群膳食暴露安全指数IAPS均小于1.【结论】研究结果为鸡蛋中氯霉素残留液相色谱-串联质谱测定提供了依据,也为北京市鸡蛋中氯霉素膳食暴露风险评估提供了参考.

【Objective】To understand the residue behavior and possible dietary exposure risk of chloramphenicol in eggs of Beijing,a rapid multi-residue analytical method for chloramphenicol residue determination in eggs was developed and validated using solid phase extraction(SPE)and ultra-high performance liquid chromatography with tandem mass spectrometry(UPLC-MS/MS).【Method】The samples were analyzed by the UPLC-MS/MS on a reversed phase C_(18) column using a gradient elution program with 0.1%aqueous formic acid and 0.1%methanol formic acid as the mobile phase.The target analyses were quantified by internal standard method.【Result】The LOD and LOQ of chloramphenicol were 0.008μg/kg and 0.02μg/kg,ranging from 0.1μg/L to 5μg/L chloramphenicol.There was a good linear relationship between the mass concentration and the corresponding peak area,and the correlation coefficients were higher than 0.9995.The IAPS for chronic risk were less than 1 for the people age of 3-6,and 20-69 with chloramphenicol in eggs.【Conclusion】The result provided a basis and reference for the detection of chloramphenicol in eggs and the risk assessment of chloramphenicol in eggs for Beijing.