毛细管气相色谱法测定盐酸莫西沙星中有机溶剂的残留量

Determination of Residual Organic Solvents in Moxifloxacin Hydrochloride by Capillary GC

目的采用毛细管气相色谱法测定盐酸莫西沙星原料药中6种有机溶剂的残留量。方法采用毛细管气相色谱法,DB-624色谱柱,程序升温,以二甲基亚砜为溶剂,进样口温度为200℃,FID检测器温度为250℃,载气流速为2.0m L·min-1,对甲醇、丙酮、乙腈、二氯甲烷、四氢呋喃和三乙胺的残留量进行检测。结果 6种有机溶剂基本实现基线分离且线性关系良好(r均在0.9990以上);甲醇、丙酮、乙腈、二氯甲烷、四氢呋喃和三乙胺的检测限分别为0.98,0.81,0.50,2.14,0.40,0.61μg·mL^(-1);平均回收率为92.06%~99.77%,RSD为1.6%~3.0%(n=9)。结论该法适用于盐酸莫西沙星中这6种有机溶剂残留量的测定。

OBJECTIVE To determine six residual organic solvents in moxifloxacin hydrochloride by capillary gas chromatography （GC）. METHODS The capillary gas chromatography was used with a DB-624 column, pro- grammed temperature, DMSO as the solvent to determine methanol, acetone, acetonitrile, dichloromethane, tetrahydro- furan and triethylamine, the inlet temperature was 200℃ and the FID detector temperature was 250℃, the flow rate of carrier gas was 2. 0mL·min^-1. RESULTS The six organic solvents were separated and showed good linear rela- tionship （ r 〉 0. 9990 ）. The detection limit of methanol, acetone, acetonitrile, dichloromethane, tetrahydrofuran and triethylamine was 0. 98,0. 81,0. 50,2. 14,0. 40,0. 61μg·mL^-1, respectively;The average recovery rate was ranged from 92. 06% to 99.77% with RSD of 1.6% -3.0% （n =9）. CONCLUSION The developed method is suitable for the quality control of the six residual organic solvents in moxifloxacin hydrochloride.