顶空气相色谱法测定盐酸厄洛替尼中有机溶剂残留量  

Determination of Residual Organic Solvents in Erlotinib Hydrochloride by Headspace Gas Chromatography

作　　者：杨琪 刘延新 纪红英 姜鹰雁 杨海霞 

机构地区：[1]山东省药学科学院,山东省生物药物重点实验室,济南250101 [2]山东福瑞达医药集团公司,山东省黏膜与皮肤给药技术重点实验室

出　　处：《中国药师》2016年第6期1198-1200,共3页China Pharmacist

基　　金：“重大新药创制”科技重大专项(编号:2009ZX09301-013)

摘　　要：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 headspace capillary gas chromatography method for the determination of residual solvents in erlotinib hydrochloride. Methods： A DB-624 capillary column （30 m ×0.53 mm, 3.0μm） was used and the carrier gas was nitro- gen. The flow rate was 2.0 ml · min -1 and the inlet temperature was 190℃. The FID detector temperature was 230 ℃. The column temperature program was with the initial temperature of 35℃ （maitaining 8 min）, risen to 170℃ with the rate of 28℃ · min-l（main- taining 8 min）, and then risen to 200℃ with the rate of 32℃ ·min-1 （maintaining 7 min）. The headspace vial temperature was 100 ℃ and the time was 30 min. Results： Ethanol, isopropanol, methylene chloride and n-butanol had a good linear relationship within the range of 0.68-409.14 μg· m1-1 （r =0.999 8） ,0.67-404.88 μg · m1-1 （r =0.999 8） ,1. 71-51. 3μg · m1-1 （r =0.999 7） and 0.72-431.12 μg · m1-1 （r =0.999 8）, respectively. The average recovery was 99.0% （RSD =0.41%, n =9）, 100.2% （RSD = 0.52%, n = 9） ,97.1% （RSD = 1.75%, n = 9） and 102.5% （RSD = 1.08%, n = 9 ）, respectively. Conclusion： The method is simple and accurate, which can be used for the determination of four residual organic solvents in erlotinib hydroehloride.

关 键 词：盐酸厄洛替尼 有机溶剂残留量 顶空气相色谱法 

分 类 号：R927.11[医药卫生—药学]