Hygiene Detection Center, School of Public Health and Tropical Medicine, Southern Medical University, Guangzhou 510515, China; Department of Pharmacy, Nanfang Hospital, Southern Medical University, Guangzhou 510515, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2013 Nov 15;939:86-91. doi: 10.1016/j.jchromb.2013.09.019. Epub 2013 Sep 23.
A rapid, sensitive, and selective ultra fast liquid chromatography-tandem mass spectrometry method was developed for quantitative determination of arenobufagin in rat plasma. Sample pretreatment involved a one-step protein precipitation with methanol using 0.1mL rat plasma. The separation was carried out on a Shim-pack XR-ODS II (75mm×2.0mm, i.d. 2.1μm) column with gradient elution at a flow rate of 0.30mLmin(-1). The mobile phase was acetonitrile and 0.1% formic acid in water. A post-column switching valve was applied to reduce the matrix effect. The detection was performed on a triple-quadruple tandem mass spectrometer in the multiple reaction monitoring mode after electrospray ionization. Linear calibration curves for arenobufagin were obtained over the concentration range 1.056-1056ngmL(-1), with a lower limit of quantification of 1.056ngmL(-1). The intra-day and inter-day precision values were lower than 15% and the accuracy ranged from 5.4% to 9.8% at all quality control levels. The method was successfully applied to the determination and pharmacokinetic study of arenobufagin in rat plasma following intraperitoneal administration.
建立了一种灵敏、快速、选择性的超高效液相色谱-串联质谱法，用于定量测定大鼠血浆中的蟾毒灵。样品预处理采用甲醇一步蛋白沉淀法，用 0.1mL 大鼠血浆。分离在 Shim-pack XR-ODS II（75mm×2.0mm，内径 2.1μm）柱上进行，以 0.30mLmin(-1)的流速进行梯度洗脱。流动相为乙腈和水中的 0.1％甲酸。在后柱切换阀的作用下，降低了基质效应。电喷雾电离后，采用三重四极串联质谱仪在多反应监测模式下进行检测。蟾毒灵在 1.056-1056ngmL(-1)浓度范围内呈线性，定量下限为 1.056ngmL(-1)。日内和日间精密度均低于 15%，所有质控水平的准确度范围为 5.4%至 9.8%。该方法成功应用于腹腔注射后大鼠血浆中蟾毒灵的测定和药代动力学研究。
