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
韦锦宁 1王雅雯 1叶煌杰 1罗恒真1
作者信息
- 1. 江西科睿药业有限公司,江西赣州 341000
- 折叠
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,0.25 μm),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7.5 µg/mL,在质量浓度7.5～100µg/mL范围内线性关系良好,10～100 µg/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.
Abstract
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,0.25 μm)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 1 μL.The limit of quantitation of(S)-(+)-Glycidyl butyrate is 7.5 μg/mL,the method was linear from 7.5 μg/mL to 100 µg/mL,the accuracy was 96.2％～103.1％in three concentration levels from 10 µg/mL to 100 µg/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Key words
GC/(R)-(-)-Glycidyl butyrate/enantiomer/analytical validation引用本文复制引用
出版年
2024
NETL
NSTL
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