鹿茸保健品中11种性激素的气相色谱-串联质谱法分析

建立了气相色谱-串联质谱法测定鹿茸保健品中11种性激素的分析方法。鹿茸中的性激素经固相萃取富集和净化,经七氟丁酸酐衍生处理。采用DB-5色谱柱(30 m×0.25 mm, 0.25 μm)、非线性梯度升温程序分离,在串联质谱多反应监测(MRM)模式下检测,外标法定量,实现了11种性激素的有效分离。11种性激素的检出限为1.0～5.0 μg/kg,线性相关系数为0.9916～0.9999,平均回收率为67.4%～99.1%,相对标准偏差为2.6%～13%。该方法准确,可靠,可满足鹿茸保健品中性激素含量的测定和确证。

Simultaneous determination of eleven sex hormones in antler velvet health products by gas chromatography-tandem mass spectrometry

A method for the simultaneous determination of 11 sex hormones in antler velvet health products by gas chromatography-tandem mass spectrometry (GC-MS/MS) was developed. The sex hormones in antler velvet were enriched and purified by solid phase extraction and derivatized with heptafluorobutyric acid anhydride (HFBA). A DB-5 column (30 m x 0.25 mm, 0.25 microm) with nonlinear gradient program was used in GC separation. The sex hormones were determined in the multiple reaction monitoring mode. The method realized the complete separation of 11 sex hormones. The limits of detection of this method were from 1.0 to 5.0 microg/kg for the 11 sex hormones. The correlation coefficients were between 0.991 6 and 0.999 9. The recoveries were in the range of 67.4% - 99.1% with relative standard deviations (RSDs) of 2.6% - 13%. This method is accurate and reliable for the determination of the sex hormones in antler velvet health products.