气相色谱法测定舒必利原料药中甲醇、乙醇的残留量  

Determination of Methanol and Ethanol in Sulpiride by GC

作　　者：张文凯 梁中卫 王兰[1] 任干 Zhang Wenkai;Liang Zhongwei;Wang Lan;Ren Gan(Jiangsu Tasly Diyi Pharmaceutical Co.,Ltd.,Huaian 223003;Huaian Huaice Technology Co.,Ltd.,Huaian 223003,China)

机构地区：[1]江苏天士力帝益药业有限公司,江苏淮安223003 [2]淮安淮测科技有限公司,江苏淮安223003

出　　处：《广东化工》2021年第15期232-232,227,共2页Guangdong Chemical Industry

摘　　要：目的:建立气相色谱法测定舒必利原料药中甲醇、乙醇残留量。方法:以DB-624(30 m×0.53 mm×3.0μm)为色谱柱,程序升温;氮气为载气;流速为每分钟4.0 m L;检测器为FID检测器,检测器温度为250℃;进样口温度为140℃;进样量为1μL;分流比为5∶1。结果:甲醇在2.068~310.2μg/m L范围内线性关系良好(r=0.999),乙醇在4.132~619.8μg/m L范围内线性关系良好(r=0.999);甲醇回收率为99.7%,RSD为0.63%;乙醇回收率为100.8%,RSD为0.83%。结论:本方法测定舒必利原料药中甲醇、乙醇的残留量,方法灵敏、准确,优于现有检测方法,有利于提高药品的安全性。Objective: To establish a GC method to determination of methanol and ethanol in sulpiride. Methods: The A DB-624 column(30 m*0.53 mm*3.0 μm)(temperature programming), nitrogen as carrier gas(flow rate: 4.0 m L·min-1) and FID detector(temperature: 250 ℃) were used. Injection port temperature was140 ℃, injection volume was 1 μL and the split ratio was 5∶1. Results: The calibration curves were well linear for methanol and ethanol in the range of 2.068~310.2μg/m L(r=0.999) and 24.132~619.8 μg/m L(r=0.999), respectively. The recovery of methanol and ethanol were 99.7 %(RSD=0.63 %) and 100.8 %(RSD=0.83 %),respectively. Conclusion: The method is sensitive, accurate, precise and reliable to determine of methanol and ethanol in sulpiride, which is superior to other methods,and good for improving the safety of drug.

关 键 词：舒必利 甲醇 乙醇 残留溶剂 气相色谱法 

分 类 号：TQ[化学工程]