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建立高效液相色谱-串联质谱(LC-MS/MS)测定动物血浆中罗匹尼罗浓度的方法。血浆经乙酸乙酯萃取后,以HPLC分离,电喷雾离子化(ESI~+)串联质谱检测。以甲醇-乙腈-0.1‰冰醋酸(36:9:55)为流动相,流速为0.2mL·min~(-1),采用Ultimate XB-C 18柱(150mm×2.1mm,3μm)分离,在三级四极杆串联质谱中经电喷雾电离源(ESI)离子化,以多反应监测(MRM)方式进行检测。盐酸罗匹尼罗、盐酸苯海拉明(内标)的扫描离子对m/Z分别为261→114和m/Z 256→167。LC-MS/MS测定血浆中罗匹尼罗线性范围为0.02—400ng·mL~(-1),范围内线性关系良好(r=0.9998);以3个浓度水平的质量控制样品求得各浓度水平日内、日间精密度(RSD)均小于15.2%。在非临床药代动力学研究中,应用此法测定了受试兔子血浆中罗匹尼罗的浓度。该法灵敏、快速、准确,操作简便,样品处理方便,线性范围宽,该方法检测快速、专一、灵敏,可满足罗匹尼罗临床前药代动力学研究和临床药动学研究的要求。
To establish a method for the determination of ropinirole concentration in animal plasma by high performance liquid chromatography-tandem mass spectrometry (LC-MS / MS). After the plasma was extracted with ethyl acetate, it was detected by HPLC and electrospray ionization (ESI ~ +) tandem mass spectrometry. The separation was performed on a Ultimate XB-C 18 column (150 mm × 2.1 mm, 3 μm) using methanol-acetonitrile-0.1% glacial acetic acid (36: 9:55) as mobile phase with a flow rate of 0.2 mL · min -1 Three-stage quadrupole mass spectrometry ionization by electrospray ionization source (ESI), detected by multiple reaction monitoring (MRM). Scanning ion pairs of ropinirole hydrochloride and diphenhydramine hydrochloride (internal standard) were 261 → 114 and m / Z 256 → 167, respectively. The linear range of ropinirole in plasma was 0.02-400 ng · mL -1 by LC-MS / MS, and the linearity was good (r = 0.9998). The three concentrations of ropinirole During the day, the precision of daytime (RSD) was less than 15.2%. In non-clinical pharmacokinetic studies, this method was used to determine the concentration of ropinirole in the plasma of test rabbits. The method is sensitive, rapid, accurate, easy to operate, convenient for sample processing and wide linear range. The method is rapid, specific and sensitive and can meet the requirements of preclinical pharmacokinetics and clinical pharmacokinetics of ropinirole .