毛细管气相色谱法测定奥美沙坦酯中14种有机溶剂的残留量

Determination of fourteen kinds of organic residual in olmesartan medoxomil by capillary gas chromatography

目的:采用高效毛细管气相色谱法,溶液直接进样法测定奥美沙坦酯原料药中甲醇、乙醇、乙醚、丙酮、乙腈、二氯甲烷、正己烷、异丙醚、醋酸乙酯、氯仿、二氧六环、甲苯、二甲基甲酰胺和二甲苯等14种有机溶剂的残留量,并进行方法学的研究。方法:采用6%氰丙基苯基,94%二甲基聚硅氧烷毛细管色谱柱(30m×0.53 mm,涂层厚3μm),程序升温的色谱条件,以二甲亚砜为溶剂,直接进样测定。结果:甲醇、乙醇、乙醚、丙酮、乙腈、二氯甲烷、正己烷、异丙醚、醋酸乙酯、氯仿、二氧六环、甲苯、二甲基甲酰胺和二甲苯呈良好的线性关系。平均回收率良好,最小检测限分别为0.4、0.4、1.6、1.2、0.7、2.0、0.5、1.5、0.8、3.3、0.6、0.3、2.8 ng和0.8 ng。结论:本方法可用于奥美沙坦酯中甲醇等14种有机溶剂的残留量的检测,灵敏度高,重复性好。

Objective：To establish by capillary gas chromatography for the analysis of organic residual in olmesartan medoxomil by direct injection of solution, and compare with the results. Methods： Wide-bore capillary column （30m × 0.53mm） packed with 6% eyanopropylphenyl-94% dimethylpoly-siloxane（ deep film 3μm ）was used on a programmed column temperature. DMSO was used as solvent, and samples were injected for the analysis. Results：The calibration curves of methanol,ethanol,ether,aeetone,aeetonitrile,diehloromethane, n-hexane,isopropylether, ethyl acetate, chloroform, dioxane, toluene, dimethylformamide and xylene showed good linearity. The average recoveries were good. The detection limits were 0.4 ng ,0.4 ng, 1.6 ng, 1.2 ng,0.7 ng,2.0 ng,0.5 ng, 1.5 ng,0.8 ng, 3.3 ng ,0.6 ng ,0.3 ng ,2.8 ng 和10.8 ng , respectively. Conclusion： The results showed that the method can be used to detect the organie residual in olmesartan medoxomil, the method have high sensitivity and good repetition.