CAJ | 학술논문

目的：建立同时测定地西泮及其代谢产物质量浓度的HPLC－MS／MS方法。方法色谱柱：Kromasil C18，流动相：乙腈－2 mmol? L－1乙酸铵水溶液（70∶30），流速：0．3 mL? min－1，柱温：40℃，用正离子扫描，多反应监测方式测定样品中药物的质量浓度。考察该方法的专属性、标准曲线和定量下限、精密度与回收率、基质效应及稳定性。结果肝微粒体孵育样品中，地西泮在20～1000 ng? mL－1线性关系良好（ r＞0．99），定量下限为20 ng? mL－1。去甲地西泮、替马西泮和奥沙西泮在2～100 ng? mL－1线性关系良好（ r＞0．99），定量下限为2 ng? mL－1。地西泮、去甲地西泮、替马西泮和奥沙西泮绝度回收率分别在55．47％～68．76％，64．84％～79．11％，68．32％～78．27％和72．66％～83．82％，日内与日间精密度均小于15％。结论本研究方法简便、快速、准确，适用于测定肝微粒体孵育样品中地西泮及其代谢产物的浓度。
목적：건립동시측정지서반급기대사산물질량농도적HPLC－MS／MS방법。방법색보주：Kromasil C18，류동상：을정－2 mmol? L－1을산안수용액（70∶30），류속：0．3 mL? min－1，주온：40℃，용정리자소묘，다반응감측방식측정양품중약물적질량농도。고찰해방법적전속성、표준곡선화정량하한、정밀도여회수솔、기질효응급은정성。결과간미립체부육양품중，지서반재20～1000 ng? mL－1선성관계량호（ r＞0．99），정량하한위20 ng? mL－1。거갑지서반、체마서반화오사서반재2～100 ng? mL－1선성관계량호（ r＞0．99），정량하한위2 ng? mL－1。지서반、거갑지서반、체마서반화오사서반절도회수솔분별재55．47％～68．76％，64．84％～79．11％，68．32％～78．27％화72．66％～83．82％，일내여일간정밀도균소우15％。결론본연구방법간편、쾌속、준학，괄용우측정간미립체부육양품중지서반급기대사산물적농도。
Objective To establish a HPLC-MS/MS method for simul-taneous determination of diazapam and its three metabolites in human liv-er microsomal.Methods Kromasil C18 column was used at 40 ℃, and the mobile phase was a mixed system consisting of acetonitrile -2 mmol? L-1 mammonium acetate ( 70 ∶30 ) and a flow rate of 0.3 mL? min -1 .The detection of the samples was made using positive ion scan and multiple reaction monitoring mode.The specificity, linearity and limit of quantification, precision and recovery, matrix effect and sta-bility were assessed.Results The sample showed good linearity from 20-1000 ng? mL-1 ( r>0.99 ) and the lower limit of quantitation was 20 ng? mL-1 .The liner calibration curve of nordiazepam, temazepam and oxazepam obtained concentration range of 2 -100 ng? mL-1 (r>0.99) and the low limit of quantitation was 2 ng? mL-1 .The average recovery rates of diazepam, nordiazepam, temazepam and oxaze-pam were 55.47% to 68.76%, 64.84% to 79.11%, 68.32% to 78.27%and 72.66%to 83.82%.The intra-day and inter-day relative standard deviations were both less than 15%.Conclusion The method is simple, rapid and accurate, suitable for measuring the concentration of diazapam and its three metabolites in human liver microsomal.