柱前衍生化气相色谱法测定α-乙基-2-氧代-1-吡咯烷乙酸光学异构体

Pre-column derivatization GC determination for optical isomers of α-ethyl-2-O-1-pyrrolidinylacetic acid

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 GC with pre-column derivatization method for determination of optical purity in synthetic （S）-α-ethyl-2-O-1-pyrrolidinylacetic acid,to set up quality control of α-ethyl-2-O-1-pyrrolidinylacetic acid in production process.Methods：Methanol and SOCl2 were used as derivatization reagents.The separation was carried out on an HP chiral 10% cyclodextrin column（ 30 m×0.25 mm×0.25 μm）;highly pure N2 was adopted as carrier gas at the flow rate of 1 mL·min-1;the temperature for inlet port and the FID detector were both 250 ℃;the column temperature was 120-180 ℃ and raised by program;the split ratio was 15：1;the injection amount was 0.6 μL.Result：α-ethyl-2-O-1-pyrrolidinylacetic acid has good linear relationship in the concentration range of 0.2-4.0 mg· mL-1 （ r=0.999 ）;the detection limit（S/N=3）was 5.3 μg·mL-1;the quantitative limit（S/N=10）was 20.1 μg·mL-1;each of optical isomers was well isolated.Conclusion：This method is accurate,reliable,sensitive and suitable for optical isomer control in the synthetic process of （S）-α-ethyl-2-O-1-pyrrolidinylacetic acid.