顶空毛细管气相色谱法测定右旋佐匹克隆残留量

Determination of residual organic solvents in Eszopiclone by headspace capillary gas chromatography

目的建立顶空毛细管气相色谱法测定右旋佐匹克隆中甲醇、丙酮、乙酸乙酯残留量的方法。方法采用ZB-5气相毛细管色谱柱(30m×0.53mm×3μm);FID检测器;柱温采用程序升温:起始温度40℃,维持6min,再以20℃.min-1速率升至200℃,维持10min,进样口温度130℃;检测器温度230℃;载气为N2,流速为3mL.min-1;分流比:1∶5;进样量:1mL;DMSO为溶解介质。结果甲醇、丙酮、乙酸乙酯分别在14.91～303.12、25.14～500.40和25.20～503.24μg.mL-1浓度范围内,与峰面积线性关系良好(r>0.99),检测限分别为1.52、0.71、1.26μg.mL-1;平均回收率分别为100.8%(RSD=3.6%)、99.54%(RSD=3.1%)和98.5%(RSD=3.2%)。结论该方法经济、简便;经方法学验证,灵敏度、准确度均达到有机残留的检测要求,适合用于右旋佐匹克隆残留溶剂的检测。

OBJECTIVE To determine a headspace capillary gas chromatography method for the determination of residual organic solvents（methanol,acetone,ethyl acetate） in Eszopiclone.METHODS The residual organic solvents were determined by GC with ZB-5 capillary column（30m×0.53mm×3μm）,with FID detector,the injection port temperature was maintaining at 130℃ and that of the detector at 230℃.The initial column temperature was 40℃,maintaining it for 6min,then raising the temperature to 200℃ at a rate of 20℃·min-1 and maintaining it at 200℃ for 10min.The flow rate of N2 was 3 mL·min-1.The headspace injection was applied with the injection volume of l mL and the split ratio was set at 1∶5.DMSO was used as solvent media.RESULTS The calibration curves of methanol,acetone,ethyl acetate were linear in the concentration range of 14.91～303.12,25.14～500.40 and 25.20～503.24μg·mL-1,respectively.The LOQ of methanol,acetone,ethyl acetate were 1.52,0.71 and 1.26μg·mL-1.The average recoveries（n=9） of methanol,acetone,ethyl acetate were 100.8%（RSD=3.6%）,99.5%（RSD=3.1%） and 98.5%（RSD=3.2%）,respectively.CONCLUSION This method is economy and simple,the method proved to be sensitive and accurate.It is suitable for determination of organic solvents and in Eszopiclone.