超高效液相色谱-串联质谱法测定多巴丝肼片中右旋多巴的含量  

Determination of Dextra-dopa in Madopar using ultra-performance liquid chromatography-tandem mass spectrometry

作　　者：巴春丹 王彦[1] BA Chundan;WANG Yan(School of Pharmacy,Shanghai Jiaotong University,Shanghai 200240,China)

机构地区：[1]上海交通大学药学院,上海200240

出　　处：《分析试验室》2024年第11期1636-1640,共5页Chinese Journal of Analysis Laboratory

摘　　要：以2,3,4,6-四乙基-O-乙酰基-β-D-吡喃葡萄糖基异硫氰酸酯(GITC)为柱前衍生试剂,建立了超高效液相色谱-串联质谱法(UPLC-MS/MS)检测多巴丝肼片中右旋多巴(D-多巴)的方法。样品经水(含1 mol/L盐酸)和N-甲基吡咯烷酮(NMP)提取后,GITC衍生,采用电喷雾正离子(ESI^(+))模式和多反应监测(MRM)模式,内标法定量。结果显示,D-多巴在0.75~10.75μmol/L (0.08%~1.08%)范围内线性关系良好,相关系数(r)为0.9949,方法定量限为0.75μmol/L (0.08%)。在0.50μg/mg (0.05%),1.00μg/mg (0.10%)和1.50μg/mg (0.15%)添加水平下,D-多巴的平均回收率为95.2%~104.4%,相对标准偏差(RSDs)为1.3%~3.2%。该方法适用于多巴丝肼片中D-多巴杂质的分析检测要求。A novel method has been developed for the quantification of Dextra-dopa (D-dopa) in Madopar by utilizing ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with 2,3,4,6-tetraO-acetyl-β-D-glucopyranosyl isothiocyanate (GITC) as pre-column derivative reagent.The sample was extracted with 1 mol/L HCl aqueous solution and N-methyl pyrrolidone (NMP),followed by derivatization with GITC,and subsequent analysis using UPLC-MS/MS.The ionization was carried out in electrospray positive ionization (ESI~+) mode employing multiple reaction monitoring (MRM).Quantification was achieved by an internal standard curve.The obtained results demonstrated a good linear correlation coefficient (r) of 0.9949 in a concentration range of 0.75 to 10.75μmol/L (0.08%-1.08%),with the quantitation limit of 0.75μmol/L (0.08%).Upon spiking the samples at three levels of 0.50μg/mg (0.05%),1.00μg/mg (0.10%) and 1.50μg/mg (0.15%),the average recoveries of D-dopa ranged from 95.2% to 104.4%,with the relative standard deviations (RSDs) ranging from 1.3% to 3.2%.This method is suitable for the accurate determination of D-dopa in Madopar samples.

关 键 词：右旋多巴 多巴丝肼片 2 3 4 6-四乙基-O-乙酰基-β-D-吡喃葡萄糖基异硫氰酸酯(GITC) 超高效液相色谱-串联质谱法(UPLC-MS/MS) 

分 类 号：O658.1[理学—分析化学]