奥沙拉秦钠残留溶剂测定方法的改进

目的：改进奥沙拉秦钠残留溶剂的测定方法。方法：采用气相色谱顶空进样,色谱柱为DB-624弹性毛细管柱,柱温：110℃;检测器：FID;进样口温度：200℃,检测器温度：250℃;载气：N2;流速：3.0 ml·min-1;分流进样;分流比：1∶1,以水为溶剂测定二氯乙烷,三氯甲烷残留量。结果：两种残留溶剂能够完全分离,二氯乙烷,三氯甲烷分别在0.25~2.52（r=0.999 5）,2.28~22.84μg·ml-1（r=0.999 5）范围内,线性关系良好,平均回收率分别为98.4%,99.5%,RSD分别为1.14%和1.78%（n=9）。最低检出限分别为0.02,0.06μg·ml-1。结论：该顶空气相色谱法准确可靠,灵敏度高,可用于奥沙拉秦钠中残留溶剂的测定。

Improvement of Determination Method for Residual Organic Solvents in Olsalazine Sodium

Objective： To improve the determination method for the residual solvents in olsalazine sodium. Methods： 1,2-Dichloroethane and chloroform were determined by headspace GC with a DB-624 capillary column and an FID detector. The column temperature was 110℃. The temperature of the injector and the detector was 200℃ and 250℃,respectively. The carrier gas was nitrogen with a flow of 3. 0 ml·min- 1. The split ratio was 1∶ 1. Water was used as the solvent. Results： 1,2-Dichloroethane and chloroform were completely separated with good linearity within the respective range of 0. 25-2. 52（ r = 0. 999 5） and 2. 28-22. 84 μg · ml- 1（ r =0. 999 5）. The average recoveries were 98. 4% and 99. 5% with RSD of 1. 14% and 0. 98%（ n = 9）,respectively. The detection limit were 0. 02 and 0. 06 μg·ml- 1,respectively. Conclusion： The method is rapid,sensitive and accurate,which can be used in the determination of residual organic solvents in olsalazine sodium.