University of California, Davis, 2921 Stockton Boulevard, Suite 1630, Sacramento, CA 95817, United States of America.
California State University, Sacramento, 6000 J Street, Sacramento, CA 95819, United States of America.
J Chromatogr B Analyt Technol Biomed Life Sci. 2018 Oct 1;1096:228-235. doi: 10.1016/j.jchromb.2018.08.016. Epub 2018 Aug 21.
A novel UPLC-UV method was developed for analysis of timolol in human plasma using a simple, fast, and cost effective ion-exchange SPE procedure, followed by separation on a C UPLC column with a mobile phase consisting of acetonitrile, phosphate buffer, and sodium 1-octane sulfonate as an ion pairing agent. The method was fully validated according to US-FDA guidelines, and was found to be sufficiently accurate and precise for analysis of timolol in human plasma for clinical pharmacokinetic studies. The application of ion-exchange SPE cartridges for purification of timolol in plasma produced excellent percent recoveries and good sample clean-up, while the ion-pairing separation described here allowed quantitation of timolol without interference from endogenous sample components. The method lower limit of detection was 1.7 ng/mL and the lower limit of quantitation was 5.0 ng/mL, allowing for analysis of therapeutic concentrations of timolol in plasma.
建立了一种新型的 UPLC-UV 法，用于分析人血浆中的噻吗洛尔，采用简单、快速、经济有效的离子交换 SPE 方法，然后在 C UPLC 柱上用包含乙腈、磷酸盐缓冲液和 1-辛烷磺酸钠的流动相进行分离，作为离子对试剂。该方法根据美国 FDA 指南进行了全面验证，结果表明，该方法对于临床药代动力学研究中分析人血浆中的噻吗洛尔是足够准确和精确的。用于血浆中噻吗洛尔纯化的离子交换 SPE 小柱的应用产生了出色的回收率和良好的样品净化效果，而此处描述的离子对分离允许定量分析噻吗洛尔，而不受内源性样品成分的干扰。该方法的检测限为 1.7ng/mL，定量限为 5.0ng/mL，允许分析治疗浓度的噻吗洛尔在血浆中。
