气相色谱法测定化合物中R-氯甘油的含量

Detection of(R)-(-)-3-Chloro-1,2-Propanediol in Compounds by Gas Chromatography

建立了气相色谱法测定化合物中R-氯甘油含量的方法.试验条件:FID检测器,检测器温度为290℃;进样口温度280℃,分流比1∶1;载体为氮气,流速5 mL/min;柱温初始温度75℃,保持3 min,以20℃/min的升温速率上升到150℃,再以8℃/min的升温速率上升到180℃,以30℃/min的升温速率上升到240℃,并维持12.5 min.试验结果:空白溶剂不干扰测定,R-氯甘油峰与其他残留溶剂峰分离度良好,检测限为2.06 ng,定量限为6.58 ng,方法专属、灵敏.在80~200μg/ml范围内,R-氯甘油浓度与峰面积的线性关系良好,线性方程为y=2.5588 x-62.469,线性回归系数r为0.9994.同一溶液连续进样6次,结果之间的RSD低于1.0%,方法进样精密度良好.同一均质样品平行测定6份,结果之间的RSD低于1.5%,方法重复性良好.加样回收率结果均介于98%~102%之间,方法准确度良好.方法适用于胆碱类物质中R-氯甘油含量的测定.

A method to determine(R)-(-)-3-Chloro-1,2-propanediol in compounds by gas chromatography(GC)is set up.With the FID detector temperature:290℃,inlet temperature:280℃,split ratio 1∶1,carrier gas:N 2,flow rate:5 mL/min.The column temperature program:initial temperature 75℃hold for 3 min,heat up to 150℃at a rate of 20℃/min,and then heat up to 180℃at a rate of 8℃/min,at last heat up to 240℃at a rate of 30℃/min and hold for 12.5 min.The blank solution had no interference on the solvents to be tested,(R)-(-)-3-Chloro-1,2-propanediol peak was well separated from other residual solvent peaks,so the specificity was good.The LOQ was 2.06 ng,the LOD was 6.58 ng,and the linearity was acceptable.The linear relationship between(R)-(-)-3-Chloro-1,2-propanediol concentration and peak area,in the range of 80~200μg/mL was good,linear equation:y=2.5588 x-62.469,correlation coefficient r was 0.9994.The same solution has been injected continuously for 6 times,and the RSD among the results was less than 1.0%.The RSD of the same homogenous sample was less than 1.5%,so the method reproducible.All the results of spiked recovery were in the range of 98%~102%,so the method is accurate.The method is suitable for testing(R)-(-)-3-Chloro-1,2-propanediol in choline.