基于UPLC-MS技术的拉坦前列素滴眼液中15S-拉坦前列素分析

发布时间：2018-08-17 19:31

【摘要】：目的:建立超高效液相色谱-四极杆-静电场轨道阱高分辨质谱法定量检测拉坦前列素滴眼液中15S-拉坦前列素。方法:采用色谱柱Thermo Accucore-C_(18)(2.1mm×150 mm,2.6μm);流动相为甲醇-乙腈-水(用冰乙酸调节p H3.0)(48∶12∶40);流速为0.3 m L·min~(-1);柱温为35℃;进样量为10μL。采用HESI离子源,正离子扫描模式,扫描范围为m/z 300~600。采用Full MS模式提取离子方式检测,拉坦前列素与15S-拉坦前列素的检测离子均为[M+Na]~+m/z 455.277±0.003;电喷雾离子源雾化温度为300℃;毛细管电压为3.50 k V;离子传输管温度为320℃。鞘气为50 arb;辅助气为10 arb;分辨率为(R)70 000。结果:15S-拉坦前列素质量浓度在0.998 8~19.98 ng·m L~(-1)范围内线性关系良好,相关系数为r=0.999 8,平均回收率为96.8%(n=9);定量限为0.029 96 ng·m L~(-1);3批样品中15S-拉坦前列素的含量分别为0.11%、0.24%、0.06%。结论:经方法学验证,本方法可检测拉坦前列素滴眼液中15S-拉坦前列素立体异构体杂质。
[Abstract]:Objective: to establish a high performance liquid chromatography-tetrapole-electrostatic field trap high resolution mass spectrometry (HRMS) method for the determination of 15 S- lattanprost in lattanprost eye drops. Methods: the mobile phase of Thermo Accucore-C18 (2.1mm 脳 150mm-1) was methanol-acetonitrile-water (adjusted with glacial acetic acid) (48:12:40), the flow rate was 0.3 mL 路min ~ (-1), the column temperature was 35 鈩，

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