顶空毛细管气相色谱法同时测定磷酸特地唑胺原料药中4种有机溶剂的残留量  

Simultaneous determination of four types of residual organic solvents in the tedizolid phosphate raw material by headspace capillary GC

作　　者：吕丹 唐克慧 王宇弛 张春然 王瑛瑛 张静霞 王术兰 Lu Dan;Tang Ke-hui;Wang Yu-chi;Zhang Chun-ran;Wang Ying-ying;Zhang Jing-xia;Wang Shu-lan(Sichuan Industrial Institute of Antibiotics,Chengdu University,Chengdu 610052)

机构地区：[1]成都大学四川抗菌素工业研究所,成都610052

出　　处：《中国抗生素杂志》2019年第1期101-105,共5页Chinese Journal of Antibiotics

摘　　要：目的建立同时测定磷酸特地唑胺原料药中甲醇、二氯甲烷、乙酸乙酯和二氧六环4种有机溶剂残留量的方法。方法采用顶空毛细管气相色谱法。色谱柱为DB-624毛细管柱,检测器为氢火焰离子化检测器(FID),柱温采用程序升温(初始温度50℃,保持5min,以15℃/min的速度升温至220℃,再保持5min),进样口温度为200℃,检测器温度为250℃,载气使用高纯氮气,流速为3.0mL/min,分流比设置为5:1,顶空瓶温度设置为100℃,平衡时间设定为30min,顶空进样体积为1.0mL。结果甲醇、二氯甲烷、乙酸乙酯和二氧六环4种有机溶剂峰之间的分离度符合要求,线性关系良好(r≥0.9990),定量限分别为0.5716、0.8190、0.3625和0.6133μg/mL,检测限分别为0.1715、0.2457、0.1087和0.1840μg/mL;精密度试验的RSD<2.0%,稳定性、重复性试验中只检出甲醇,RSD<2.0%;平均回收率在97.12%～104.83%范围内,RSD分别为0.92%、1.64%、0.70%和1.72%,3批磷酸特地唑胺原料药检测结果均符合限度要求。结论该方法快速、灵敏、准确,适用于磷酸特地唑胺原料药中残留溶剂的检测。Objective To establish a method for simultaneous determination of four types of residual organic solvents in the tedizolid phosphate raw material, namely methanol, dichloromethane, ethyl acetate, and 1,4-dioxane. Methods Headspace capillary gas chromatography was adopted. The determination was performed on DB-624 capillary column using the temperature programming. The temperature of injector port was 200 ℃ , and the flame ionization detector was used with the temperature of 250 ℃ . Nitrogen was used as the carrier gas with a flow rate of 3.0mL/min. The spilt ratio was 5:1, and the head-space injection volume was 1.0mL. The head-space equilibrium temperature was set at 100 ℃ , and the equilibrium time was 30min. Results The linear ranges of methanol, dichloromethane, ethyl acetate and 1,4-dioxane were well separated, and a good linearity was obtained within the designed range for each solvent with the correlation coefficients no less than 0.9990. The limits of quantitation were 0.5716, 0.8190, 0.3625 and 0.6133μg/mL;the limits of detection were 0.1715, 0.2457, 0.1087 and 0.1840μg/mL, respectively. RSD of the precision test was lower than 2.0%. Only methanol was detected in the stability test and reproducibility tests, RSD < 2.0% . The average recoveries were from 97.12% to 104.83%, RSD were 0.92%, 1.64%, 0.70% and 1.72%, respectively. All the residual solvents in tedizolid phosphate were within the limited quantity range.Conclusions The method is rapid, sensitive, and accurate for the content determination of residual solvents in the tedizolid phosphate raw material.

关 键 词：顶空毛细管气相色谱法 磷酸特地唑胺 有机溶剂 残留量 

分 类 号：R917[医药卫生—药物分析学]