LC-MS法测定(1R,2R)-1,2-双(甲磺酰基氧基甲基)环己烷的对映异构体杂质

Determination of Enantiomer of(1R,2R)-1,2-Bis(methanesulfonyloxymethyl)cyclohexane by LC-MS

目的:建立了一种LC-MS法测定(1R,2R)-1,2-双(甲磺酰基氧基甲基)环己烷的对映异构体杂质的方法。方法:采用表面键合直链淀粉-三(3-氯-5-甲基氨基甲酸酯)的硅胶为填充剂(大赛璐IG-U 100×3.0 mm,1.6μm);以0.1%甲酸水溶液-甲醇(30︰70,体积比)为流动相;流速为0.3 mL/min;柱温为35℃;进样体积为2μL;采用岛津LCMS检测,前体离子为323.0274。结果:(1R,2R)-1,2-双(甲磺酰基氧基甲基)环己烷的对映异构体的线性范围为0.05%~0.6%水平的杂质,相关系数为0.999;检测限为0.01%水平的杂质,定量限为0.03%水平的杂质,具有较高的检测灵敏度;平均回收率为95.3%,RSD为4.1%,准确度高,精密度高;微小改变色谱条件(柱温、流动相比例和流速)的检测结果好,耐用性好。结论:建立的检测方法准确、灵敏,适合于(1R,2R)-1,2-双(甲磺酰基氧基甲基)环己烷的异构体的测定。

Objective:To establish an LC-MS method for determination of enantiomer of(1R,2R)-1,2-bis(methanesulfonyloxymethyl)cyclohexane.Methods:The analytical column wassilica gel bonded with amylose-tris(3-chloro-5-methylphenylcarbamate)column(DAICEL IG-U 100×3.0 mm,1.6μm).Mobile phase was 0.1%formic acid aqueous solutionmethanol(70∶30,volume ratio).The flow rate was 0.3 mL/min.The column temperature was 35℃.Shimadzu LCMS,precursor ion was 323.0274.The injection volume was 2μL.Results:The linear ranges was 0.05%~0.6%,correlation coefficient was 0.999.The detection limit was 0.01%and the quantitative limit was 0.03%,high sensitivity.The average recovery was 95.3%,RSD was 4.1%,high accuracy and precision.The detection result was good by changing the micro chromatographic conditions(column temperature,flow comparison and flow rate),the assessment of the robustress was good.Concusion:This method was accurate,sensitive and reliable to determine enantiomer of(1R,2R)-1,2-bis(methanesulfonyloxymethyl)cyclohexane.