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[摘要]
目的:利用 GC / MS 技术建立测定口服舒心平软胶囊后人血浆样品中龙脑含量的方法。方法:采用 HP-WAX 石英毛细管柱(30 m × 0.25 mm × 0.25 μm),柱温为 150 ℃,保持 5.5 min,以 40 ℃/min 的速率升至 190℃,保持 1 min。以氦气为载气,分流比为 5∶1,扫描方式选择离子检测(SIM),定量龙脑为m/z 95,定量内标(萘)为m/z 128。结果:龙脑和内标的保留时间分别为 4.56 min 和 5.31 min,龙脑在 5~1 000 ng/mL线性关系良好(r = 0.999 3),高、中、低 3 个浓度的样品提取回收率均在 80 % 以上。结论:本测定方法可以快速简便地定量分析人血浆样品中的龙脑含量,有较高的灵敏度和较好的重现性,可以满足舒心平的人体药代动力学研究。
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[Abstract]
Objective: A sensitive and selective GC/MS method has been developed to determine the level of borneol in human plasma after po ShuXinPing Capsules. Methods: The quantitative analysis were carried out by using a HP-WAX silica capillary column(30 m × 0.25 mm × 0.25 μm). The column was maintained at 150 ℃ for 5.5 min, then the temperature was increased to 190 ℃ which was kept for 1 min at the speed of 40 ℃/min. Helium was applied as carrier gas. The splitting-ratio was 5∶1. Selective ion monitoring(SIM)was utilized for quantitation of the molecules. Borneol was monitored for the ion of m/z 95, while ions of m/z 128 were selected for naphthalene(IS). Results: The reserve time of borneol and IS was 4.56 min and 5.31 min, respectively. Linearity was tested ranging from 5 to 1 000 ng/mL(r = 0.999 3). The average recoveries were 86.7 %, 81.9 % and 83.9 % at the concentrations of 10, 50 and 500 ng/mL. Conclusion: The method is simple, fast, high sensitive and repeatability for quantitative analysis of borneol in human plasma, which was applied in pharmacokinetics research of ShuXinPing Capsule.
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