基于UPLC-MS技术的拉坦前列素滴眼液中15S-拉坦前列素分析  

Analysis of 15S-latanoprost in latanoprost eye drops by UPLC-Q-orbitrap mass spectrometer

作　　者：胡立新 

机构地区：[1]临沂市食品药品检验检测中心,临沂276000

出　　处：《药物分析杂志》2017年第11期2031-2037,共7页Chinese Journal of Pharmaceutical Analysis

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。Objective： To determine 15S-latanoprost in latanoprost eye drops by UPLC-Q-orbitrap mass spectrometer. Methods： The separation was carried out on an Thermo Accucore-Cls （ 2.1 mm × 150 mm, 2.6 μm ） column with the mobile phase consisting of methanol - acetonitrile-water （ pH was adjusted to 3.0 with acetic acid ） （ 48 ： 12 ： 40 ）, the flow rate was 0.3 mL·min-1 and the column temperature was 35 ℃, and the injection volume was 10 μL. HESI was employed, the sample was analyzed in the positive mode, with the probe heater temperature at 300 ℃, capillary temperature 320 ℃, and m/z range was from 300 to 600, and detected at [M＋Na]＋ m/z 455.277 ~ 0.003 for both latanoprost and 15 S-latanoprost. Results： The calibration curve of 15S-latanoprost was a good linear/ty within concentration range of 0.998 8-19.98 ng· mL-1, and the correlation coefficients was 0.999 8. The limits of 15S-latanoprost was 0.029 96 ng· mL-1, the average recovery of 15S-latanoprost was 96.8% （ n=9 ）. The contents of 15S-latanoprost in 3 batches of samples were 0.11%, 0.24%, 0.06% respectively. Conclusion： The methodology validation proved that the method is useful as a quality control method for trace analysis of 15S-latanoprost in latanoprost eye drops.

关 键 词：拉坦前列素 15S-拉坦前列素 液相色谱-质谱联用 差向异构体 杂质分析 

分 类 号：R917[医药卫生—药物分析学]