顶空-气相色谱法测定硫酸长春地辛中残留溶剂的含量  

Residual solvents content of vindesine sulfate determined by headspace gas chromatography method

作　　者：李咏华 黄程程 林秀仙 

机构地区：[1]广州白云山汉方现代药业有限公司,广州501970

出　　处：《中国当代医药》2015年第23期7-10,共4页China Modern Medicine

摘　　要：目的 建立顶空-气相色谱法测定硫酸长春地辛中残留溶剂甲醇、乙醇、丙酮、二氯甲烷、三氯甲烷、四氢呋喃含量的方法。方法 采用聚乙二醇毛细管柱（DB-WAX）,以FID为检测器,柱初始温度45℃保持10 min后升温至220℃,载气为氮气,流速为1.0 ml/min。结果 甲醇在60-360μg/ml范围内,线性关系良好（r=0.9997）,平均回收率为98.00%,RSD为1.30%;乙醇在100-600μg/ml范围内,线性关系良好（r=0.9997）,平均回收率为99.44%,RSD为1.67%;丙酮在100-600μg/ml范围内,线性关系良好（r=0.9999）,平均回收率为97.31%,RSD为2.23%;二氯甲烷在12-72μg/ml范围内,线性关系良好（r=0.9989）,平均回收率为97.05%,RSD为2.59%;三氯甲烷在1-8μg/ml范围内,线性关系良好（r=0.9978）,平均回收率为99.17%,RSD为4.62%;四氢呋喃在15-90μg/ml浓度范围内,浓度与峰面积呈现良好的线性关系（r=0.9998）,平均回收率为95.19%,RSD为2.00%。结论 本法简便,准确度好,灵敏度高,可用于硫酸长春地辛中残留溶剂的含量测定。Objective To establish the method of headspace gas chromatography determinating the residual solvents content in vindesine sulfate such as methanol,ethanol,acetone,methylene chloride,chloroform,tetrahydrofuran. Methods Polyethylene glycol capillary column（DB-WAX） was used and FID was used as detector.The column temperature was enhanced to 220℃ after keeping the column initial temperature at 45℃ for 10 min.Nitrogen was used as carrier gas and its flow velocity was 1.0 ml/min. Results The linear relationship was good in the range from 60 μg/ml to 360 μg/ml（r=0.9997）,average recovery rate was 98.00% and RSD was 1.30%.The linear relationship was good in the range from 100 μg/ml to600 μg/ml for ethanol（r=0.9997）,average recovery rate was 99.44% and RSD was 1.67%.The linear relationship was good in the range from 100 μg/ml to 600 μg/ml for acetone（r=0.9999）,average recovery rate was 97.31% and RSD was2.23%.The linear relationship was good in the range from 12 μg/ml to 72 μg/ml for methylene chloride（r=0.9989）,average recovery rate was 97.05% and RSD was 2.59%.The linear relationship was good in the range from 1 μg/ml to 8 μg/ml for chloroform（r=0.9978）,average recovery rate was 99.17% and RSD was 4.62%.The linear relationship was good in the range from 15 μg/ml to 90 μg/ml（r=0.9998）,average recovery rate was 95.19% and RSD was 2.00%. Conclusion This method is simple and has good accuracy and high sensitivity,which can be used for determination the residual solvents content in vindesine sulfate.

关 键 词：硫酸长春地辛 顶空-气相色谱法 残留溶剂 

分 类 号：R657.71[医药卫生—外科学]