基于UPLC-MS技术的拉坦前列素滴眼液中15S-拉坦前列素分析.docVIP

基于UPLC-MS技术的拉坦前列素滴眼液中15S-拉坦前列素分析 胡立新 临沂市食品药品检验检测中心 X 关注成功！ 加关注后您将方便地在 我的关注中得到本文献的被引频次变化的通知！ 新浪微博 腾讯微博 人人网 开心网 豆瓣网 网易微博 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-C18 (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 300600。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0.998 819.98 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。 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; 作者简介：胡立新 Tel: (0539) 8056520;E-mail:443068611@ 收稿日期：2017年1月3日 Analysis of 15S-latanoprost in latanoprost eye drops by UPLC-Q-orbitrap mass spectrometer HU Li-xin Linyi Institute for Food and Drug Control; Abstract： Objective:MTo determine 15S-latanoprost in latanoprost eye drops by UPLC-Q-orbitrap mass spectrometer.ethods:The separation was carried out on an Thermo Accucore-C18 (2.1 mm×150 mm, 2.6μm) column with the mobile phase consisting of methanol–acetonitrile-water (p H was adjusted to 3.0 with acetic acid) (48∶12∶40) , the flow rate was 0.3 m L·min-1 and the column temperature was 35℃, and the injection volume was 10μL.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 linearity 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·m L-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.Concl