GC-MS/MS稳定同位素稀释技术测定蜂蜜中的氯霉素

Determination of Chlormphenicol(CAP) Content in Honey by GC-MS/MS using Stable Isotope Dilution Technique

[目的]建立稳定同位素稀释技术测定蜂蜜中氯霉素（CAP）分析方法。[方法]用氘代氯霉素（D5-CAP）为内标物,以SPC C18固相微萃取小柱净化样品,BSTFA＋TMCS为衍生剂,应用GC-MS/MS中多离子选择模式（MRM）定性及定量分析。[结果]该法在0.46-9.22 ng内线性良好,相关系数为0.9965,加标回收率79.8%-102%。当称样量为5.0 g时,最低检定浓度为0.02μg/kg。该方法参加国际食品分析能力测试蜂蜜中氯霉素的测定考核,结果满意。[结论]GC-MS/MS稳定性同位素稀释法具有方法稳定、定性定量准确及灵敏度高的优点,可用于蜂蜜中氯霉素测定。

[Objective] To determine the content of Chloramphenicol （CAP） in honey using stable isotope dilution technique. [Methods] Using deuterium Chloramphenicol （D5-CAP） as internal standard, using SPC C18 solid phase minim extraction column to cleanse the sample and BSTFA＋TMCS to make it derived. The sample was analyzed qualitatively and quantitatively using much ion choice mode （MRM） method by GC-MS/MS. [Results] There was a good linearity within 0.46 ng-9.22 ng, and the correlation coefficient was 0. 9965 and additional standard recovery rate was 78.9%-102%. When the content of additional standard was 5.0g, the least concentration was 0.02μg/kg. The method passed the assess the content determination of CAP in honey by the Food Analysis Performance Assessment Scheme （FAPAS）. [Conclusion] Stable isotope dilution technique with GC-MS/MS is a stable method, showing exact qualitative and quantitative results and high sensitivity for determining the content of CAP in honey.