采用液相色谱-串联质谱法测定畜禽肉中维生素D3和25-OH-D3的含量。样品经过皂化,固相萃取净化,正相制备后,Symmetry C18色谱柱分离,采用大气压化学电离源多反应监测模式检测。氘代维生素D3作为内标物。维生素D3和25-OH-D3的线性范围均为5~100 μg·L-1,检出限(3S/N)均为0.60 μg·kg-1。方法用于猪肉样品的分析,加标回收率在75.0%~97.1%之间,测定值的相对标准偏差(n=6)在1.9%~5.6%之间。

LC-MS/MS was applied to the determination of vitamin D3 and 25-hydroxy vitamin D3 in poulty. After saponification,SPE purification and positive phase preparation of the sample,symmetry C18 chromatographic column was used for separation,and APCI and multi-reactions monitor were adopted in MS/MS. Deuterated vitamin D3 was used as internal standard. Linearity ranges of vitamin D3 and 25-hydroxy vitamin D3 were found in the same range of 5-100 μg·L-1 with same detection limits (3S/N) of 0.60 μg·kg-1. The proposed method was applied to the analysis of pork sample,giving values of recovery and RSD′s (n=6) in the ranges of 75.0%-97.1% and 1.9%-5.6%,respectively.