固相萃取-气相色谱-质谱法测定二羟丙茶碱中痕量3-氯-1,2-丙二醇

SPE/GC-MS determination of 3-mono-chloropropane-1,2-diol residue in diprophylline

目的:建立二羟丙茶碱中痕量3-氯-1,2-丙二醇(3-MCPD)的气相色谱-质谱联用定性定量方法。方法:试样经饱和氯化钠提取,弗罗里硅土层析柱分离净化,旋转蒸发浓缩,三氟乙酸酐衍生后,进行气相色谱-质谱联用(SIM模式)检测。结果:3-氯-1,2-丙二醇在10～500μg·kg-1范围呈良好线性关系(r=0.9993,n=5),检出限为2.3μg·kg-1,三水平加标回收率均在96%以上,RSD在0.249%～1.151%之间。结论:该方法灵敏度高,重现性好,适用于药品中痕量3-氯-1,2-丙二醇的测定。

Objective：A new method for the determination of 3-Mono-chloropropane-1,2-diol residue in diprophylline was established.Methods：The sample was preseparated with a magnesium trisilicate.3-Mono-chloropropane-1,2-diol residue was derivatizated with Trifluoroacetic acid anhydride and determined by gas chromatography-mass spectrometry（GC-MS） with the single-ion monitoring mode.Results：The linearity over the concentration range 10-500 μg·kg-1（r=0.9993,n=5） was obtained.the detection limit of 3-MCPD was 2.3 μg·kg-1,the recovery rate was over 96%.The relative standard deviation of the precision and the reproducibility for the proposed method were 0.389% and 0.252%.Conlusion：The method is fast and sensitive,can be used it to analyze trace 3-MCPD in medicines.