顶空气相色谱法测定地屈孕酮原料药中的6种有机溶剂残留  

Determination of Six Organic Solvent Residues in Active PharmaceuticalIngredients of Dydrogesterone Drug by HS-GC

作　　者：邹明慧 Zou Minghui(School of Pharmacy,Jiangsu Ocean University,Lianyungang 222000,China)

机构地区：[1]江苏海洋大学药学院,江苏连云港222000

出　　处：《山东化工》2024年第12期116-119,123,共5页Shandong Chemical Industry

摘　　要：目的:建立测定地屈孕酮原料药中残留溶剂的顶空气相色谱法(Head space-gas chromatography,HS-GC)。方法:采用6%氰丙基苯基-94%二甲基聚硅氧烷为固定液的毛细管柱为色谱柱(DB-624,30 m×0.53 mm,膜厚3.00μm),程序升温,检测器为氢火焰离子化检测器,温度为240℃,进样口温度为200℃,载气为氮气,流速为2 mL/min,分流比为10∶1,顶空进样,进样量为1μL。结果:乙醇、丙酮、正己烷、二氯甲烷、乙酸乙酯和异丙醚定量限质量浓度分别为5.2220,5.3620,0.5929,0.2942,5.1840,5.2420μg·mL^(-1),检测限质量浓度分别为1.5666,1.6086,0.1779,0.0883,1.5552,1.5726μg·mL^(-1),在测定浓度范围内有良好的线性,相关系数(r)均大于0.990,平均回收率分别为105.06%,102.02%,106.78%,100.13%,100.99%,103.06%。结论:该检测方法操作简单,经方法学验证,适用于检测地屈孕酮中6种残留溶剂的残留量。Objective:To establish a gas chromatography to measuring residual solvents in dydrogesterone drug substance.Methods:The capillary column with 6%cyanopropyl phenyl-94%dimethylpolysiloxane as fixative is chromatography column(DB-624,30 m×0.53 mm,film thickness 3.00μm),the procedure heating,temperature of flame ionization detector is 240℃,inlet temperature is 200℃,carrier gas is nitrogen,flow rate is 2 mL/min,shunt ratio is 10∶1,top space injection sample is 1μL.Results:The quantitative limit concentrations of ethanol,acetone,N-hexane,dichloromethane,ethyl acetate and isopropanether were 5.2220,5.3620,0.5929,0.2942,5.1840,5.2420μg·mL^(-1),respectively,Detection limit concentrations were 1.5666,1.6086,0.1779,0.0883,1.5552,1.5726μg·mL^(-1),respectively,Have a good linearity in the measured concentration range,The correlation coefficient(r)is greater than 0.990,The average recovery rates were 105.06%,102.02%,106.78%,100.13%,100.99%and 103.06%,respectively.Conclusion:The detection method is easy to operate and suitable to detect the residual amount of 6 residual solvents in dydrogesterone.

关 键 词：顶空气相色谱法 地屈孕酮 残留溶剂 

分 类 号：TQ460[化学工程—制药化工]