Department of Applied Therapeutics, Faculty of Pharmacy, Kuwait University, Kuwait.
J Sep Sci. 2010 Jul;33(13):1888-96. doi: 10.1002/jssc.200900800.
A rapid LC-MS/MS method for quantification of an enaminone analog, E121 in mouse plasma using E118 as an internal standard (IS) has been developed and validated. The analyte was analyzed on C(18) column using a mobile phase of acetonitrile/methanol/ammonium acetate/formic acid (60:20:20:0.025, v/v/v/v) at a flow rate of 0.25 mL/min. Quantitation was achieved using ESI+ interface, employing MRM mode at m/z 308>262 and 222>194 for E121 and IS, respectively. The calibration standards were linear over a range of 0.10-20 microg/mL (r(2)>0.99) with an LLOQ of 0.1 microg/mL (RSD%; 11.4% and bias%; 9.5%). Intra- and inter-run precision of E121 assay ranged from 3.7 to 10.9% with accuracy (bias) that varied between -10.0 and 12.0%, demonstrating good precision and accuracy. Recoveries of E121 and the IS from plasma were above 80%. Stability of E121 in plasma showed that the analyte was stable under various conditions. The matrix effect study showed a lack of effect. The applicability of the developed method was demonstrated by measuring E121 in mouse plasma samples following intraperitoneal administration of various doses ranging from 10 to 100 mg/kg and this study demonstrates that E121 exhibits linear kinetics in the dose range studied.
一种快速的 LC-MS/MS 方法，用于定量分析小鼠血浆中的烯胺酮类似物 E121，使用 E118 作为内标 (IS)。该分析物在 C(18)柱上使用乙腈/甲醇/乙酸铵/甲酸 (60:20:20:0.025，v/v/v/v) 作为流动相，流速为 0.25 mL/min。通过 ESI+接口，采用 MRM 模式，在 m/z 308>262 和 222>194 处分别对 E121 和 IS 进行定量。校准标准在 0.10-20 µg/mL 范围内呈线性 (r(2)>0.99)，LLOQ 为 0.1 µg/mL (RSD%; 11.4%和偏差%;9.5%)。E121 测定的日内和日间精密度范围为 3.7-10.9%，准确度 (偏差) 在-10.0 和 12.0%之间，表明精密度和准确度良好。E121 和 IS 从血浆中的回收率均高于 80%。E121 在血浆中的稳定性表明，该分析物在各种条件下均稳定。基质效应研究表明无影响。该方法的适用性通过测量腹腔内给予 10-100 mg/kg 不同剂量后小鼠血浆样品中的 E121 得到证明，该研究表明 E121 在研究剂量范围内呈线性动力学。
