气相色谱法测定尼可地尔原料药中乙二醇的残留量  

Determination of Ethanediol in Nicorandil 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17期174-175,共2页Guangdong Chemical Industry

摘　　要：目的:建立气相色谱法测定尼可地尔原料药中乙二醇残留量。方法:以DB-WAXETR(30 m×0.53 mm×1.0μm)为色谱柱,程序升温;氮气为载气;流速为每分钟5.0 mL;检测器为FID检测器,检测器温度为260℃;进样口温度为140℃;进样量为1μL;分流比为10∶1。结果:乙二醇在6.389~76.668μg/mL范围内线性关系良好(r=0.9991),回归方程为Y=0.593X-0.8867;回收率为98.28%,RSD为4.3%;检出限为0.62μg/mL,定量限为6.2μg/mL。结论:本方法测定尼可地尔原料药中乙二醇的残留量,方法灵敏、准确,有利于提高药品的安全性。Objective:To establish a GC method to determination of ethanediol in nicorandil.Methods:A DB-WAXETR column(30 m*0.53 mm*1.0μm)(temperature programming),nitrogen as carrier gas(flow rate:5.0 mL·min-1)and FID detector(temperature:260℃)were used.Injection port temperature was 140℃,injection volume was 1μl and the split ratio was 10∶1.Results:The calibration curve was well linear for ethanediol in the range of 6.389~76.668μg/mL(r=0.9991).The recovery of ethanediol was 98.28%(RSD=4.3%).The LOD was 0.62μg/ml and the LOQ was 6.2μg/mL.Conclusion:The method is sensitive,accurate,precise and reliable to determine of ethanediol in nicorandil,and good for improving the safety of drug.

关 键 词：尼可地尔 乙二醇 质量控制 残留溶剂 气相色谱法 

分 类 号：TQ[化学工程]