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

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10～500 μg·kg^-1范围呈良好线性关系（r=0.9993, n=5）,检出限为2.3 μg·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.