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□A rapid and sensitive analytical method of liquid chromatography combined with tandem mass spectrometry (LC–MS/MS) was established for simultaneous quantitative analysis of hydrazine, methylhydrazine, and 1,1-dimethylhydrazine in rat plasma. Plasma samples were pretreated with protein precipitation and optimized derivatization procedure. Separation was achieved using acetonitrile and water containing 5 mM ammonium acetate as gradient elution. The optimized mass transition ion-pairs (m/z) monitored for three hydrazine derivatives werem/z299.1→m/z151.1,m/z180.2→m/z78.1, andm/z194.2→m/z59.1, respectively. The lower limit of quantitation (LLOQ) of hydrazine was 1 ng/mL and those of other compounds were 10 ng/mL. Intra- and inter-day precision were within 14.00%. Meanwhile, the relative error was within the acceptable range. The recovery of three analytes and (IS) were between 57.78 ± 4.73%and 107.04 ± 7.46%.Target derivatives were stable under the conditions tested. The dilution test showed that this method is not only suitable for samples in the detection limit but also applicable for high concentration samples that exceed the upper limit of detection. The performance of the method was successfully verified for real rat plasmas and would be useful for routine analysis in cases of suspected hydrazine poisoning. [ABSTRACT FROM AUTHOR]

A highly selective and sensitive liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed for the quantification of scicinib, a novel thiosemicarbazone analogue and anticancer agent in rat plasma. Protein precipitation with saturated EDTA solution and methanol was selected for sample preparation, and brodimoprim was employed as the internal standard (IS). The analytes were separated on a Symmetry C18column (200 × 4.6 mm i.d., 5 µm) by isocratic elution with a mobile phase consisting of methanol and 0.2 mM EDTA (75:25, v/v) at a flow rate of 0.4 mL/min. After electrospray ionization, the analyte and IS were recorded under selected reaction monitoring (SRM) mode. The chosen transition wasm/z313.0 → 267.9 for scicinib andm/z339.0 → 280.9 for IS, respectively. The validated linearity range is 5–5000 ng/mL, with the lower limit of quantitation of 5 ng/mL. The developed method was successfully applied to a pharmacokinetic study of scicinib in rats after a single intravenous administration of 5 mg/kg. [ABSTRACT FROM AUTHOR]