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目的:建立手性色谱柱拆分血浆和尿液中那格列奈对映体（D-那格列奈和L-那格列奈）的简便方法。方法:采用Chiralcel OD-R （10μm,0.46cm×25cm）手性色谱柱,流动相为乙腈-0.5mol·L-1高氯酸钠（70:30）,0.5mol·L-1高氯酸调pH2.2,检测波长214nm,流速:0.4mL·min-1,内标法室温测定。结果:血浆中D-那格列奈的线性范围是0.02～20mg·L-1,r=0.9995;L-那格列奈的线性范围是0.08～20mg·L-1,r=0.999 4 ;尿液中D-那格列奈的线性范围是0.02～10mg·L-1,r=09998;L-那格列奈的线性范围是0.08～10mg·L-1,r=0.9997;血浆中D-那格列奈高中低3个质控样品的日内RSD≤6.9％,日间RSD≤8.2％,L-那格列奈高中低3个质控样品的日内RSD≤7.1％,日间RSD≤10.0％;尿液中D-那格列奈高中低3个质控样品的日内RSD≤7.0％,日间RSD≤9.8％,L-那格列奈高中低3个质控样品的日内RSD≤7.3 ％,日间RSD≤10.3％。结论:本方法分离度好,简便快速,完全适用于D-那格列奈人体药代动力学及肝代谢过程中消旋化的研究。
Objective: To establish a convenient method for the separation of enantiomers of nateglinide (D-nateglinide and L-nateglinide) in plasma and urine by chiral column. Methods: Chiralcel OD-R (10μm, 0.46cm × 25cm) was used as the mobile phase. The mobile phase was acetonitrile-0.5mol·L-1 sodium perchlorate Adjust pH2.2, detection wavelength 214nm, flow rate: 0.4mL · min-1, internal standard method for determination of room temperature. Results: The linear range of D-nateglinide in plasma was 0.02 ~ 20 mg · L-1, r = 0.9995. The linear range of L-nateglinide was 0.08 ~ 20 mg · L-1, r = 0.999 4. The linear range of D-nateglinide in liquid was 0.02-10 mg · L-1, r = 09998; the linear range of L-nateglinide was 0.08-10 mg · L-1, r = 0.9997; The intra-day RSD≤6.9% of three quality control samples of nateglinide high and low, RSD≤8.2% day, RSD≤7.1% of the three quality control samples of L-nateglinide high and low, daytime RSD≤10.0 %. The intra-day RSD≤7.0% of three quality control samples of D-nateglinide in urine and the daytime RSD≤9.8%, the intra-day RSD of three quality control samples of L-nateglinide high and low≤7.3 %, Daytime RSD≤10.3%. Conclusion: This method has good resolution, simple and rapid, and is fully suitable for the study of human pharmacokinetics and D-galactosyl-racemization in D-nateglinide.