顶空进样气相色谱法测定醋酸布舍瑞林微球中二氯甲烷残留量

Determination of Dichloromethane Residue in Buserelin Acetate Microspheres by Headspace Gas Chromatography

目的建立顶空进样气相色谱法测定醋酸布舍瑞林微球中二氯甲烷的残留量。方法采用顶空气相色谱法,ZB-624毛细管色谱柱(30 m×0.53 mm,3μm),氢火焰离子化检测器,载气为氮气,外标法计算含量。结果在考察的浓度范围内,线性关系良好(r=0.999 8);回收率为99.6%~105.5%,RSD为1.8%(n=9)。结论经方法学验证,该方法准确度高,重复性好,可用于检测醋酸布舍瑞林微球制剂中残留的二氯甲烷。

Objective To establish a method for determination of dichloromethane residue in buserelin acetate microspheres.Methods Gas head-space chromatography was applied to this study.The column was ZB-624 capillary column(30 m×0.53 mm,3μm),the carrier gas was nitrogen and the detector was FID.The content of dichloromethane residue was determined by the external standard method.Results All the calibration curves showed good linearity(r=0.9998)over the test concentration.The overall recoveries were ranged from 99.6%-105.5%,with RSD of 1.8%(n=9).Conclusion This method is simple,flexible and with good repeatability,which can be used for determination of dichloromethane residue in buserelin acetate microspheres.