气相色谱法测定(R)-(-)-缩水甘油丁酯对映异构体的方法学研究  

GC Analysis and Methodology Research for Enantiomer in(R)-(-)-Glycidyl Butyrate

作　　者：韦锦宁 王雅雯 叶煌杰 罗恒真 WEI Jinning;WANG Yawen;YE Huangjie;LUO Hengzhen(Jiangxi Kerui Pharmaceutical Co.,Ltd.,Ganzhou 341000,China)

机构地区：[1]江西科睿药业有限公司,江西赣州341000

出　　处：《山东化工》2024年第20期156-159,162,共5页Shandong Chemical Industry

摘　　要：建立气相色谱法用于测定(R)-(-)-缩水甘油丁酯中的对映异构体((S)-(+)-缩水甘油丁酯),该方法用氢火焰离子化检测器,检测器的温度设置为300℃;进样口的温度设置为220℃;使用SPB-20(体积分数20%苯基-80%二甲基聚硅氧烷)中含25%2,3-二-O-乙酰基-6-O-TBDMS-β-环糊精为固定液的毛细管柱(Supelco Beta DEX 225,30 m×0.25 mm,0.25μm),起始柱温60℃,维持时间为3 min,升温速率为每分钟5℃,升温至200℃,维持时间为5 min;分流比设置为50∶1;以氮气作为载气,以每分钟2.5 mL作为流速,进样体积1μL。(S)-(+)-缩水甘油丁酯定量限为7.5μg/mL,在质量浓度7.5~100μg/mL范围内线性关系良好,10~100μg/mL范围内三个质量浓度水平回收率在96.2%~103.1%范围内。本方法专属性强,灵敏度、准确度高,精密度、耐用性等良好,可用于(R)-(-)-缩水甘油丁酯的质量控制。A GC method has been established for detecting enantiomer((S)-(+)-Glycidyl butyrate)in(R)-(-)-Glycidyl butyrate.The detector is a hydrogen flame ionization detector,with a temperature set at 300℃;The temperature of injection port is 220℃;A SPB-20(20%phenyl-80%dimethylpolysiloxane)containing 25%2,3-di-O-acetyl-6-O-TBDMS-β-Capillary column with cyclodextrin as stationary liquid(Superlco Beta DEX 225,30 m×0.25 mm,0.25μm)was used.The initial column temperature is 60℃,maintained for 3 minutes,and heated at a rate of 5℃per minute to 200℃,maintained for 5 minutes;The split ratio is 50∶1;The carrier gas is nitrogen,and the flow rate is 2.5 mL per minute.The injection volume is 1μL.The limit of quantitation of(S)-(+)-Glycidyl butyrate is 7.5μg/mL,the method was linear from 7.5μg/mL to 100μg/mL,the accuracy was 96.2%~103.1%in three concentration levels from 10μg/mL to 100μg/mL.The method has strong specificity,high sensitivity and accuracy,good precision and durability,and can be used for the quality control of(R)-(-)-Glycidyl butyrate.

关 键 词：气相色谱法 (R)-(-)-缩水甘油丁酯 对映异构体 方法学 

分 类 号：O657.7[理学—分析化学]