GC-MS法测定婴幼儿奶粉中17β-雌二醇、雌三醇、炔雌醇、雌酮残留量

Determination of 17 β-Estradiol、Estriol,Ethinylestradiol,Estrone in Infant Milk with Gas Chromatography-Mass Spectrometry

通过液液萃取和固相萃取提取、净化婴幼儿奶粉中添加的雌激素17β-雌二醇、雌三醇、炔雌醇、雌酮,以DTE+MSTFA+TMIS衍生化试剂进行衍生化,气相色谱-质谱联用(选择离子模式)对衍生物检测分析,确定了样品中17β-雌二醇、雌三醇、炔雌醇、雌酮的定性和定量分析方法,该法检出限为0.5μg/kg,定量限为1.0μg/kg。衍生物的峰面积与样品浓度为0.5~1000.0μg/L呈良好的线性关系,线性回归系数均在0.999以上。各物质不同加入量的添加回收率在72.6%~92.8%,变异系数为2.3%~4.1%。该方法可实现对样品进行灵敏、准确的定性定量分析。

The residual estrogen drugs of 17β-estradiol, estriol, ethinylestradiol, estrone in infant milk were extracted and purified by the method of liquid-liquid partition and solid phase extraction. The target durgs were separated and validated by gas chromatography spectrometry(selected ion mode) after derivatization of the purified sample with the DTE+MSTFA+TMIS derivative reagent, and the qualitative and quantitative analysis method was developed. Its LOD and LOQ is 0.5 μg/L and 1.0 μg/kg, respectively. And there were a good linear correlation between the ratio of peak areas and the concentrations of drugs in the add range of 0.5~1 000.0 μg/L, the correlative coefficients were above 0.999 . The recoveries of different concentration of estrone was 72.6 %~92.8 %. The RSD of the method was between 2.3%~4.1%. The method is suitable for the qualitative and quantitative analysis of the target drugs in the infant milk.