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

朱镇星; 马密茸; 李翠杰; 罗艳; 关妮妮; 胡建伟; 金辉

doi:10.13748/j.cnki.issn1007-7693.20241286

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 Ethyl (R)-(−)-4-Cyano-3-hydroxybutyratic Acid by Pre-column Derivatization Gas Chromatography

摘要

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。
方法采用供试品的乙酸酐溶液30 mg·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(30 m×0.25 mm，0.25 μm)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，最低定量限为15 μg·mL⁻¹；对映异构体在15~225 μg·mL⁻¹内的线性关系良好(Y=0.2395x+0.2516，相关系数r=1.0000)；仪器精密度RSD为2.2%(n=6)，中间精密度RSD为2.6%(n=12)，平均回收率101.4%~108.9%；溶液常温放置3 d稳定。
结论该方法操作简便、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 To establish a pre-column derivatization gas chromatography method for detection of ethyl (R)-(−)-4-cyano-3-hydroxybutyratic acid(ATS-5) isomer.
METHODS The concentration of ATS-5 in anhydride aceic acid was 30 mg·mL⁻¹, Amberlyst-15 was added to derivatization; the Supelco Beta DEX 325(30 m×0.25 mm, 0.25 μm) 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 15 μg·mL⁻¹; the liner for ATS-5 isomer in the rang of 15−225 μg·mL⁻¹(Y=0.2395X+0.2516, r=1.0000) was good; the RSD of repeatability was 2.2%(n=6); the RSD of intermediate precision was 2.6%(n=12); the recovery was 101.4%−108.9%; the sample solution was stable at room temperature for 3 d.
CONCLUSION This method is simple, specificity, accurate and reproducible, which can detect isomer in ethy ATS-5.

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