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目的:利用柱前衍生化气相色谱法,建立(S)-α-乙基-2-氧代-1-吡咯烷乙酸制备过程中产物光学纯度的检测方法,为其合成反应过程的控制提供依据。方法:以甲醇和SOCl2为衍生化试剂,采用手性色谱柱HPChiral10%Cyclodextrin(30m×0.25mm×0.25μm),载气为N2,流速1mL.min-1,进样口温度250℃,FID检测器温度250℃,程序升温,分流比15:1,进样量0.6μL。结果:α-乙基-2-氧代-1-吡咯烷乙酸浓度在0.2～4.0mg.mL-1范围内线性关系良好(r=0.999);检测限(S/N=3)为5.3μg.mL-1;定量限(S/N=10)为20.1μg.mL-1;对映体均达到基线分离。结论:该方法准确可靠,灵敏度高,重现性好,可用于(S)-α-乙基-2-氧代-1-吡咯烷乙酸合成过程的质量控制。
OBJECTIVE: To establish a method for the determination of optical purity of (S) -α-ethyl-2-oxo-1-pyrrolidineacetic acid by precolumn derivatization gas chromatography and to provide a basis for the control of its synthesis reaction . Methods: Chiral column HPChiral10% Cyclodextrin (30m × 0.25mm × 0.25μm) was used as the derivatization reagent with methanol and SOCl2. The carrier gas was N2, the flow rate was 1mL.min-1, The temperature of the device is 250 ℃, the program temperature is increased, the split ratio is 15: 1, and the injection volume is 0.6μL. Results: The linearity of α-ethyl-2-oxo-1-pyrrolidineacetic acid was good (r = 0.999) in the range of 0.2-4.0 mg.mL-1. The detection limit (S / N = 3) .mL-1; the limit of quantitation (S / N = 10) was 20.1μg.mL-1; Conclusion: The method is accurate, reliable and reproducible. It can be used for the quality control of (S) -α-ethyl-2-oxo-1-pyrrolidineacetic acid synthesis.