CAJ | 학술논문

目的:建立快速测定人血浆中硫普罗宁浓度的HPLC-MS联用分析方法.方法:在全血中加入抗氧剂半胱氨酸后,于分得的血浆中加入霉酚酸为内标,酸化后经乙酸乙酯提取,进行HPLC-MS测定.色谱柱为Shim-pack VP-ODS C18 column (250 mm×2.0 mm,5 μm),流动相为甲醇-0.1 %乙酸(70:30),流速为0.2 mL/min.结果:方法的线性范围为30～4 000 ng/mL,提取回收率大于70%,批间和批内精密度均小于8.5%,单样品分析时间7.5 min.并将所建立的方法成功地应用于硫普罗宁片生物等效性研究.结论:本方法操作简单、快速,灵敏度、准确度、精密度和定量分析线性关系均良好,符合生物样品测定要求.
목적:건립쾌속측정인혈장중류보라저농도적HPLC-MS련용분석방법.방법:재전혈중가입항양제반광안산후,우분득적혈장중가입매분산위내표,산화후경을산을지제취,진행HPLC-MS측정.색보주위Shim-pack VP-ODS C18 column (250 mm×2.0 mm,5 μm),류동상위갑순-0.1 %을산(70:30),류속위0.2 mL/min.결과:방법적선성범위위30～4 000 ng/mL,제취회수솔대우70%,비간화비내정밀도균소우8.5%,단양품분석시간7.5 min.병장소건립적방법성공지응용우류보라저편생물등효성연구.결론:본방법조작간단、쾌속,령민도、준학도、정밀도화정량분석선성관계균량호,부합생물양품측정요구.
Aim:To develop a rapid high-performance liquid chromatography-mass spectrometry (HPLC-MS) method for the quantification of tiopronin in human plasma.Methods:Cysteine was chosen as antioxidant and firstly added into the whole blood firstly.After adding mycophenolic acid as internal standard (IS) and 1 mol/L HCl into the plasma,the samples were extracted with acetic ether and then determined by HPLC-MS.The chromatographic separation was performed on a Shim-pack VP-ODS C18 column (250 mm×2.0 mm,5 μm) using methanol-0.1% acetic acid (70∶30) as mobile phase with a flow rate of 0.2 mL/min.Results:The assay exhibited a linear range of tiopronin between 30～4 000 ng/mL.The precisions for intra- and inter-batch were all within 8.5%.The extraction recoveries were more than 70%.The total HPLC-MS analysis time was within 7.5 min per a run.The fully validated method was successfully applied to quantify tiopronin in human plasma for a bioavailability study.Conclusion:The assay proved to be accurate,sensitive,selective and convenient.The fully validated method can be applied to study the pharmacokinetics and bioavailability of tiopronin and tiopronin formulations in human.