顶空进样气相色谱法测定注射用氨曲南中4种有机溶剂的残留量

Determination of Four Residual Solvents in Aztreonam for Injection by Headspace GC

目的建立注射用氨曲南中4种有机溶剂残留量的测定方法。方法采用顶空进样毛细管气相色谱法,测定注射用氨曲南中乙醇、乙腈、四氢呋喃、N,N-二甲基甲酰胺的残留量,色谱柱为DB-624毛细管柱(60m×0.541mm,1.0μm),溶剂为二甲基亚砜,进样口温度为150℃,检测器温度220℃,氮气为载气,流量3.0mL/min。柱温为程序升温,起始温度为50℃,保持5min,以10℃/min的速率升至180℃,保持3min,再以20℃/min的速率升至200℃,保持8min。结果建立的色谱方法在所考察的质量浓度范围内线性关系良好,各溶剂回收率符合要求。结论建立的色谱方法简便灵敏,结果准确可靠,适用于注射用氨曲南中残留溶剂的检测。

Objective To establish a method for the determination of four residual solvents in aztreonam for injection. Methods To make the quantitative analysis of the residual organic solvents including ethanol, acetonitrile, tetrahydrofuran, N, N-dimethylformamide, dimethyl sulfoxide. The adopted chromatography conditions were DB-624 column （60 mm ×0. 541 mm, 1.0 μm）, dimethyl sulfoxide as solvent and FID as the detector. The injector temperature was 150 ℃, the detector temperature was 220 ℃, the flow rate of N2 was 3.0 mL/min. The column temperature was risen by program, the initial temperature was 50 ℃ keeping for 5 min, the temperature was raised to 180 ℃ at the rate of 10 ℃/min keeping for 3 rain,then the temperature was raised to 200 ℃ at the rate of 20 ℃/min, keeping for 8 min. Results The calibration curve of organic solvent residue had the good linear relationship and the recovery met the requirements. Conclusion The established method is sensitive and accurate. It can be applied to determine the organic solvent residue in aztreonam for injection.