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目的:建立顶空毛细管气相色谱法测定盐酸厄洛替尼中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(30 m×0.53 mm,3.0μm),载气为氮气,流速为2.0 ml·min~(-1),进样口温度为190℃,FID检测器温度为230℃,采用程序升温:初始温度为35℃,保持8 min,以28℃·min~(-1)升温至170℃,保持8 min,再以32℃·min~(-1)升温至200℃,保持7 min。顶空瓶平衡温度为100℃,时间30 min。结果:乙醇、异丙醇、二氯甲烷、正丁醇分别在0.68~409.14μg·ml~(-1)(r=0.999 8)、0.67~404.88μg·ml~(-1)(r=0.999 8)、1.71~51.31μg·ml~(-1)(r=0.999 7)、0.72~431.12μg·ml~(-1)(r=0.999 8)浓度范围内线性关系良好,平均回收率分别为99.0%(RSD=0.41%,n=9)、100.2%(RSD=0.52%,n=9)、97.1%(RSD=1.75%,n=9)、102.5%(RSD=1.08%,n=9)。结论:该方法简便、准确性好,适用于盐酸厄洛替尼中4种有机溶剂残留量的测定。
Objective: To establish a method for the determination of residual organic solvents in erlotinib hydrochloride by headspace capillary gas chromatography. METHODS: Headspace capillary gas chromatography was performed on a DB-624 capillary column (30 m × 0.53 mm, 3.0 μm) with a carrier gas of nitrogen at a flow rate of 2.0 ml · min -1. The inlet temperature The temperature of the FID detector was 230 ℃ and the temperature of the FID detector was 190 ℃. The initial temperature was 35 ℃ and kept for 8 min. The temperature was raised to 170 ℃ at 28 ℃ · min ~ (-1) for 8 min and then at 32 ℃ min ~ (-1) temperature was raised to 200 ℃ for 7 min. Headspace bottle equilibrium temperature of 100 ℃, time 30 min. Results: The correlation coefficients of ethanol, isopropanol, methylene chloride and n-butanol were 0.68 ~ 409.14μg · ml ~ (-1) (r = 0.999 8), 0.67 ~ 404.88μg · ml ~ (-1) (R = 0.999 7), 0.72 ~ 431.12 μg · ml -1 (r = 0.999 8), the average recoveries were 99.0% (RSD = 0.41%, n = 9), 100.2% (RSD = 0.52%, n = 9), 97.1% ). Conclusion: The method is simple, accurate and suitable for the determination of four organic solvents residues in erlotinib hydrochloride.