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建立了超高效液相色谱-四极杆-静电场轨道阱高分辨质谱法定量检测拉坦前列素(1)滴眼液中的2种立体异构体杂质——5,6-反式拉坦前列素(2)和15S-拉坦前列素(3)。采用Thermo Accucore-C_(18)色谱柱,流动相为甲醇∶乙腈∶水(用冰乙酸调至pH 3.0,48∶12∶40)。采用加热电喷雾离子源,正离子扫描模式,扫描范围m/z 300~m/z 600。采用FullMS模式检测,1、2与3的监测离子均为[M+Na]+m/z(455.277±0.003)。2、3在1~100 ng/ml范围内线性关系良好,回收率为96.50%和95.22%,RSD为1.99%和2.34%;定量限均为3 pg/ml。
A high performance liquid chromatography-quadrupole-electrostatic field orbit-trap high-resolution mass spectrometry was established for the quantitative determination of two stereoisomeric impurities in latanoprost (1) eye drops - 5,6-trans Tantamol (2) and 15S-Latanoprost (3). On a Thermo Accucore-C 18 column, the mobile phase was methanol: acetonitrile: water (adjusted to pH 3.0, 48: 12: 40 with glacial acetic acid). Using heated electrospray ion source, positive ion scanning mode, scanning range m / z 300 ~ m / z 600. Using FullMS mode detection, the monitored ions of 1, 2 and 3 were both [M + Na] + m / z (455.277 ± 0.003). 2,3 showed a good linearity in the range of 1 ~ 100 ng / ml. The recoveries were 96.50% and 95.22% with RSDs of 1.99% and 2.34%, respectively. The limits of quantification were both 3 pg / ml.