去羧氯雷他定中有机溶剂残留量检查的研究

Determination of organic residue in desloratadine

目的:测定去羧氯雷他定原料药中残留有机溶剂乙醇和乙酸乙酯的含量.方法:采用气相色谱法,顶空进样,FID检测器,以1,4-二氧六环为溶剂,异丙醇为内标,采用石英毛细管柱,以6%苯基-94%氰基丙基苯基二甲基聚硅氧烷为固定相,气化室150o C,检测器240o C,柱温65o C.结果:乙醇在10～220 μg/ml浓度范围内呈良好的线性关系(r＝0.999 9),回收率为99.03%(RSD=2.5%),最低检出限为1 μg/ml. 乙酸乙酯在10～200 μg/ml浓度范围内呈良好的线性关系(r＝0.999 9),回收率为101.5%(RSD=1.2%),最低检出限为3 μg/ml.三批去羧氯雷他定原料药中乙醇的残留量均为0.02%,乙酸乙酯的残留量均为0.03%.结论:本方法简单、快捷且灵敏度高,可用于去羧氯雷他定中乙醇和乙酸乙酯残留量的控制.

Object： To establish a method for the determination of ethanol and ethyl acetate residue in desloratadine. Methods.. A head space-GC method with 1,4-dioxane as solution and isopropanol as the internal standard was used for the determination of organic residue. The separation was performed on a quarts capillary column packed with DB-624 at 65 ℃. The injector temperature was 150 ℃ and the detector temperature was 240 ℃ with FID detector. Results： There were good linearity in the range of 10～220μg/ml （ r =0. 9999） for ethanol and 10～200μg/ml （ r =0. 9999） for ethyl acetate. Their recoveries were 99. 03% （RSD 2.5%） and 101.5% （RSD 1.2%） and detection limits were 1μg/ml and 3μg/ml, respectively. Conclusion： This method was simple, rapid and accurate. It can be used for the organic residue control of desloratadine.