摘要
目的建立保健食品中非法添加物西布曲明、N-单去甲基西布曲明质控样品的研制流程。方法采用超高效液相色谱-串联质谱法(UPLC-MS),Agilent ZORBAX SB-C18色谱柱(2.1 mm×100 mm,3.5μm),流动相缓冲液(含10 mmol/L乙酸铵和0.1%乙酸)和乙腈,电喷雾电离,多反应检测模式(MRM),对质控样品中西布曲明、N-单去甲基西布曲明进行了含量测定,并进行了方法学验证,均匀性和稳定性评价,以及不确定度的计算。结果西部曲明、N-单去甲基西布曲明的含量分别为(4.137±0.435)mg/kg、(5.033±0.545)mg/kg。结论本实验对保健食品中非法添加物西布曲明,N-单去甲基西布曲明进行了分析测量和定值,该研制流程符合相关要求,可用于质量控制样品定值的参考。
Objective To establish a development process of quality control samples for illegal addictive sibutramine and N-single demethylated sibutramine in healthy food. Methods Ultra- performance liquid chromatography- tandem mass spectrum( UPLC- MSMS) technology,Agilent ZORBAX SB- C18column( 2. 1 mm × 100 mm,3. 5 μm),mobile phase of 10 mmol / L ammonium acetate and 0. 1% acetonitrile,electrospray ionization,multi reaction detection mode( MRM) were used for the detection of sibutramine and N- single demethylated sibutramine in quality control samples,and then the methodology,homogeneity and stability test were completed. At last,the uncertainty about the results was calculated. Results The contents of sibutramine and N- single demethylated sibutramine were respectively( 4. 137 ± 0. 435) mg / kg and( 5. 033 ± 0. 545) mg / kg. Conclusion This article detected and certificated the sibutramine and N- single demethylated sibutramine in healthy food. The process matched related standards and could be used as the reference in certification of quality control samples.
出处
《中国卫生检验杂志》
CAS
2016年第21期3075-3079,3082,共6页
Chinese Journal of Health Laboratory Technology
关键词
质控样品
西布曲明
N-单去甲基西布曲明
不确定度
Quality control sample
Sibutramine
N-single demethylated sibutramine
Uncertainty