HPLC法测定人血浆中的舒芬太尼浓度

HPLC determination of sulfentanil in human plasma

目的:建立测定人血浆中舒芬太尼血药浓度的 HPLC 方法。方法:以丁丙诺啡为内标,采用正己烷-无水乙醇(19:1,v/v)进行液-液萃取。采用 Diamonsil—C_(18)柱(4.6 mm×200mm,5μm),以0.01 mol·L^(-1)KH_2PO_4-乙腈(65:35,v/v,pH 5.6)为流动相,流速为1.5 mL·min^(-1),检测波长230 nm。结果:舒芬太尼在7.8125～12500 ng·mL^(-1)范围内线性关系良好(r=0.9976),最低检测浓度为4 ng·mL^(-1)。高、中、低浓度(12500,625,31.25 ng·mL^(-1))样本方法的平均回收率均大于97%;高、中、低浓度(12500,625,31.25 ng·mL^(-1))样本日内变异分别为4.65%,6.72%,6.68%,日间变异分别为8.65%,7.49%,13.19%。结论:本方法简便,准确,稳定性好,能够满足血浆中低浓度舒芬太尼的测定及临床药代动力学研究的要求。

Objective： To establish HPLC methods for determination of sulfentanil in human plasma. Methods： Bu-prenorphin was used as an internal standard. The samples were extracted by liquid-liquid extraction method using n-hexane and ethanol （19：1,v/v）. Sulfentanil in human plasma was determined by HPLC by using Diamonsil - C18 analysisis column （4.6 mm×200 mm,5 μm）. The mobile phase of 0.01 mol·L^-1 potassium, acetonitrile （65 ：35 ,v/v ,pH 5.6） was pumed at 1.5 mL·min^-1 and the wavelength of detection was set at 230 nm. Results：The calibration curves were found to be linear in the working range between 7. 8125 to 12500 ng·mL^-1 with a good correlation （r =0. 9976）. Detection limit was 4 ng·mL^-1. The extraction recovery was more than 97%. The within-day RSD were 4.87 % ,6. 68 % ,6. 68 % respectively and the between-day RSD was 8.65 % ,8. 14 % ,13.19 % respectively. Conclusion：This method was simple and accurate for the determination of sulfentanil in human plasma and useful for pharmakinetic study of sulfentanil.