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目的建立测定大鼠血中胆碱酯酶抑制剂XQ528及其代谢物美普他酚浓度的高效液相-质谱联用法(LC-MS/MS)。方法血浆样品采用乙腈沉淀蛋白后进样测定,以尼泊金乙酯为内标。色谱柱:ZORBAX Eclipse XDB C18(50 mm×2.1mm,5μm),流动相:水(0.1%甲酸,A)-乙腈(0.1%甲酸,B),梯度洗脱,流速0.4 m L·min-1,柱温30℃,进样量20μL,总分析时间为7 min。质谱采用电喷雾离子源,以多反应离子监测模式进行定量分析。结果 XQ528及其代谢物美普他酚的线性范围分别为0.05~50μg·L-1和0.05~25μg·L-1;批内RSD分别为3.1%和9.4%,批间RSD分别为7.4%和8.6%;提取回收率分别为102.1%~103.3%和104.2%~110.0%;基质效应均在85%~115%内。结论本方法灵敏度高、准确、快速,适于大鼠血浆中XQ528及其代谢物美普他酚浓度的测定和药动学研究。
Objective To establish a high performance liquid chromatography-mass spectrometry (LC-MS / MS) method for the determination of the concentration of cholinesterase inhibitor XQ528 and its metabolite meptazalol in rat blood. Methods Plasma samples were extracted with acetonitrile and then injected into the sample, with ethylparaben as the internal standard. Column: ZORBAX Eclipse XDB C18 (50 mm × 2.1 mm, 5 μm). The mobile phase consisted of water (0.1% formic acid, A) -acetonitrile , Column temperature 30 ℃, injection volume 20μL, total analysis time 7min. Electrospray ionization mass spectrometry was used for mass spectrometry analysis in multiple reaction ion monitoring mode. Results The linear range of XQ528 and its metabolite meptazinol were 0.05-50 μg · L-1 and 0.05-25 μg · L-1, respectively. The intra-assay RSD was 3.1% and 9.4%, respectively. The inter-assay RSD was 7.4% and 8.6% %; The recoveries were 102.1% ~ 103.3% and 104.2% ~ 110.0%, respectively. The matrix effects were within 85% ~ 115%. Conclusion The method is sensitive, accurate and rapid and suitable for the determination and pharmacokinetics of XQ528 and its metabolite meptaxil in rat plasma.