CAJ | 학술논문

目的评价高效液相色谱法同时检测人血浆异丙酚和瑞芬太尼浓度的效果.方法选择健康志愿者18名,性别不限,年龄18～45岁,体重52 ～ 81 kg,采集静脉血样,采用高效液相色谱法同时检测血浆异丙酚和瑞芬太尼的浓度.以麝香草酚为内标,在血浆样品中加入0.1 mol/L的磷酸二氢钾后用正己烷∶乙酸乙酯(1∶4)萃取,以ZORBAX Eclipse XDB-C18(4.6 mm× 250.0 mm,5 μm)为色谱柱;以甲醇∶0.02 mol/L NaH2PO4∶乙腈=50∶30∶20为流动相,流速1.0 ml/min,检测波长:1～7 min用210 nm,7～ 16 min用266 nm,进样量20μl.采用最小二乘法进行线性回归分析.取瑞芬太尼低、中、高浓度(1.00、5.00、20.00 ng/ml)和异丙酚低、中、高浓度(0.50、2.00、10.00μg/ml)的血浆样品,测定回收率、精密度和稳定性.结果瑞芬太尼的直线回归方程为C=12.853 5Ai/As+0.084 8(R2=0.999 4),血浆瑞芬太尼的浓度在0.5～ 40.0 ng/ml内线性关系良好.异丙酚的直线回归方程为C=8.554 3Ai/As+ 0.029 1(R2=0.998 6),血浆异丙酚的浓度在0.2～20.0 μg/ml内线性关系良好.两者相对回收率均在85％～115％,绝对回收率大于75％,日内、日间精密度和稳定性RSD均小于5％,符合生物样品测定要求.结论本实验建立的高效液相色谱法检测灵敏度高、重现性好、快速简便,可用于人血浆异丙酚和瑞芬太尼浓度的同时检测和临床药代动力学研究.
목적 평개고효액상색보법동시검측인혈장이병분화서분태니농도적효과.방법 선택건강지원자18명,성별불한,년령18～45세,체중52 ～ 81 kg,채집정맥혈양,채용고효액상색보법동시검측혈장이병분화서분태니적농도.이사향초분위내표,재혈장양품중가입0.1 mol/L적린산이경갑후용정기완∶을산을지(1∶4)췌취,이ZORBAX Eclipse XDB-C18(4.6 mm× 250.0 mm,5 μm)위색보주;이갑순∶0.02 mol/L NaH2PO4∶을정=50∶30∶20위류동상,류속1.0 ml/min,검측파장:1～7 min용210 nm,7～ 16 min용266 nm,진양량20μl.채용최소이승법진행선성회귀분석.취서분태니저、중、고농도(1.00、5.00、20.00 ng/ml)화이병분저、중、고농도(0.50、2.00、10.00μg/ml)적혈장양품,측정회수솔、정밀도화은정성.결과 서분태니적직선회귀방정위C=12.853 5Ai/As+0.084 8(R2=0.999 4),혈장서분태니적농도재0.5～ 40.0 ng/ml내선성관계량호.이병분적직선회귀방정위C=8.554 3Ai/As+ 0.029 1(R2=0.998 6),혈장이병분적농도재0.2～20.0 μg/ml내선성관계량호.량자상대회수솔균재85％～115％,절대회수솔대우75％,일내、일간정밀도화은정성RSD균소우5％,부합생물양품측정요구.결론 본실험건립적고효액상색보법검측령민도고、중현성호、쾌속간편,가용우인혈장이병분화서분태니농도적동시검측화림상약대동역학연구.
Objective To evaluate the efficacy of high performance liquid chromatography (HPLC) for simultaneous determination of propofol and remifentanil concentrations in human plasma.Methods Methods Eighteen healthy volunteers of both sexes,aged 18-45 yr,weighing 52-81 kg,were enrolled in the study.Venous blood samples were collected,and the concentrations of propofol and remifentanil in human plasma were detected simultaneously by HPLC.The internal standard was thymol.Potassium dihydrogen phosphate 0.1 mol/L was added to the plasma and then the plasma samples were extracted with extract liquor (ethyl acetate ∶ hexane =4 ∶ 1,V/V).The analytical column was ZORBAX Eclipse XDB-C18 (4.6 mm×250 mm,5 μm).The mobile phase was methano ∶ 0.02 mol/L NaH2PO4 ∶ acetonitrile,the flow rate was 1.0 ml/min,the detection wavelength was 210 nm within 1-7 min,and 266 nm within 7-16 min,and the sample size was 20 μl.Linear regression analysis was performed by using the least-squares method.The specimens of the blood with the final concentration of remifentanil 1.00,5.00 and 20.00 ng/ml and propofol 0.50,2.00 and 10.00 μg/ml were obtained to determine the recovery,precision and stability.Results Linear regression equation of remifentanil was C=12.853 5Ai/As+0.084 8 (R2 =0.999 4),and this system showed a good linear relationship with the concentration of remifentanil ranged 0.5-40.0 ng/ml.Linear regression equation of propofol was C=8.554 3 Ai/As+0.029 1 (R2=0.998 6),and this system showed a good linear relationship with the concentration of propofol ranged 0.2-20.0 μg/ml.For both propofol and remifentanil concentrations,the relative recovery was within the range of 85％-115％,the absolute recovery was larger than 75％,and the relative standard deviation of intra-and inter-day precision and stability was less than 5％.The method was proved to meet the requirements of biological sample analysis.Conclusion For HPLC method established in this trial,the determination is sensitive,reproducible,rapid and simple,and it can be used for simultaneous determination of propofol and remifentanil concentrations in human plasma and for clinical pharmacokinetic research.