蜂蜜中磺胺类和氯霉素类同时测定的前处理方法研究

[目的]建立同时测定蜂蜜中磺胺类和氯霉素类的超高效液相色谱串联质谱(UPLC-MS)的新方法。[方法]试验以0.2%的甲酸乙腈作为提取剂,通过一种新型的小柱(OasisPRi ME HLB柱)净化处理,流动相定容过膜后上机待测,可以同时提取出蜂蜜中的磺胺类和氯霉素类。[结果]氯霉素在0.1~10.0 ng/m L范围内有良好的线性关系,相关系数大于0.991;磺胺类在0.5~50.0 ng/m L范围内线性关系良好。氯霉素样品最低检出限为0.1μg/kg,磺胺类检出限为0.5μg/kg,回收率在82.50%~101.20%,相对标准偏差为3.2%~4.0%。[结论]该方法快速、准确、灵敏度高,适用于蜂蜜中氯霉素类和磺胺类的检测。

Study on Pretreatment Method for Simultaneous Determination of Chloramphenicol and Sulfanilamide Grous in Honey

Objective] To establish a new method UPLC-MS for the determination of sulfanilamide grous and chloramphenicols in honey . [Method] With 0.2% formic acid acetonitrile as the extraction agent, through purification treatment by a new column ( Oasis? PRiME HLB), sulfanilamide grous and chloramphenicols can be extracted simultaneously.[Result] Chloramphenicol had a good linear relationship in the range of 0.1-10.0 ng/mL, and the correlation coefficient was greater than 0.991; sulfanilamide grous had a good linear relationship in the range of 0.5 -50.0 ng/mL.The lowest detection limit of chloramphenicol was 0.1 g/kg, detection limit of sulfanilamide grous was 0.5 μg/kg, recovery was 82.5%-101.2%, relative standard deviation was 3.2% -4.0%.[Conclusion] The method is rapid, accurate and sensitive, and it is suitable for the detection of chloramphenicol and sulfanilamide grous.