柱前衍生气相色谱法测定(R)-(-)-4-氰基-3-羟基丁酸乙酯的对映异构体

Analysis of the Optical Isomer of (R)-(-)-4-Cyano-3-hydroxybutyratic acid, ethyl ester by Pre-Column Derivatization Gas Chromatography.

关键词:  (R)-(-)-4-氰基-3-羟基丁酸乙酯  对映异构体  柱前衍生  Amberlyst-15  阿托伐他汀钙

Key words:  (R)-(-)-4-Cyano-3-hydroxybutyratic acid, ethyl ester  optical isomer  pre-column derivatization  amberlyst-15  atorvastatin calcium

摘要:

目的 建立一种柱前衍生气相色谱法测定(R)-(-)-4-氰基-3-羟基丁酸乙酯中对映异构体的含量。方法 本方法采用供试品乙酸酐溶液30mg·mL-1，加入Amberlyst-15催化剂进行衍生化反应，衍生物通过Supelco Beta DEX 325型色谱柱分离，用FID检测器进行检测。结果 供试品主峰与对映异构体峰之间分离度为4.1，最小检测量为15μg·mL-1，15μg·mL-1~225μg·mL-1的浓度范围内线性良好Y=0.2395x+0.2516，相关系数r=1.0000，精密度RSD=2.2%(n=6)，中间精密度RSD=2.6%(n=12)，平均回收率101.4%~108.9%，溶液常温放置3d稳定。结论 本方法操作简便，专属性良好，灵敏度高，准确度高，能够用于(R)-(-)-4-氰基-3-羟基丁酸乙酯中对映异构体检测。

Abstract:

OBJECTIVE A Pre-Column Derivatization Gas Chromatography method was established for detection of (R)-(-)-4-Cyano-3-hydroxybutyratic acid,ethyl ester isomer. METHODS The concentration of ATS-5 in anhydride aceic acid was 30mg·mL-1,Amberlyst-15 was added to derivatization;The Supelco Beta DEX 325 (30m×0.25mm×0.25μm) was used;The detector was FID. RESULTS The resolution between ATS-5 and isomer was 4.1;The quantitation limit of ATS-5 isomer was 15μg·mL-1;The liner for ATS-5 isomer in the rang of 15μg·mL-1~225μg·mL-1 (Y=0.2395x+0.2516,r=1.0000);The recovery was 101.4%~108.9%;The repeatability was RSD=2.2%(n=6),the intermediate precision was RSD=2.6%(n=12);The sample solution was stable at room temperature for 3 days. CONCLUSION This method is simple,specificity,accurate and reproducible,which can detect isomer in (R)-(-)-4-Cyano-3-hydroxybutyratic acid.