期刊文献+

固相萃取RP-HPLC法测定西达本胺血药浓度 被引量:2

Determination of Chidamide in Plasma by RP-HPLC with Solid-phase Extraction
下载PDF
导出
摘要 目的 建立测定西达本胺血药浓度的固相萃取RP-HPLC法。方法 采用Kromasil KR100-5C18(4.6mm×250mm,5μm)分析柱:柱温为室温;以0.6%醋酸水溶液.乙腈(0~6min,81:19和6—13min,76:24,v/v)为流动相,梯度洗脱;流速为1.0ml/min;紫外检测波长为260nm;以MS-275为内标,血浆样品用Waters OASIS固相萃取(SPE)小柱提取纯化,乙腈洗脱,吹干,用流动相复溶后进样分析,进样量20μl。结果 西达本胺血药浓度在0.04~10μg·ml^-1范围内线性关系良好(r=0.998 1),最低定量浓度为0.04μg·ml^-1。低、中、高3个浓度的日内RSD为5.79%~10.16%,日问RSD为2.01%~14.81%;RE为-0.85%~4.39%;平均回收率为74%。结论 此方法较简便、准确、精密度好,可以用做西达本胺的毒代动力学研究,并为临床前药代动力学研究打下了方法学基础。 Aim To establish an RP-HPLC method for the determination of Chidamide in plasma. Method The Chi-damide with the internal standard MS-275 added was extracted from the plasma with a solid-phase extraction column. Theplasma sample was loaded onto a SPE column. The Chidamide was eluted with Acetonitrile, dried by air and determinedby reversed-phase high-performance liquid chromatography(RP-HPLC) at 260nm. The mobile phase consisted of 0.6%acetic acid solution and Acetonitrile(0 ~ 6min,81:19;6 ~ 13min,76:24) with the flow rate of 1.0ml/min. The columnwas KR100-5C18(4.6mm × 250mm,5μm). The column temperature was room temperature, and the injected volume was20μl. Results The linear range was 0.04 ~ 10μg·ml^-1( r = 0.998 1 ), and the LLOQ was 0.04μg·ml^-1. The intra-dayand inter-day RSD were 2.01%(14.81% and 5.79% ~ 10.16% ,respectively. The RE was -0.85% ~ 4.39% .Theaverage extraction recovery was 74%. Conclusion The proposed method is simple, accurate and precise. It is suitable fortoxicokinetics study.
出处 《解放军药学学报》 CAS 2006年第2期113-115,共3页 Pharmaceutical Journal of Chinese People's Liberation Army
关键词 西达本胺 高效液相色谱法 固相萃取 血药浓度 Chidamide HPLC Sohd-phase extraction Plasma drug concentration
  • 相关文献

参考文献2

二级参考文献57

  • 1Ferrer I, Furlong ET. Accelerated solvent extraction followed by online solid - phase extraction coupled to ion trap LC/MS/MS for analysis of benzalkonium chlorides in sediment amples. Anal Chem,2002,4(6) :1275.
  • 2Hopfgartner G, Husser C, Zell M.High→throughput quantification of drags and their metabolites in biosamples bz LC-MS/MS and CE-MS/MS: possibilities and limitations.Ther Drug Monit,2002,4(1):134.
  • 3Zhizhina GP, Blyukhterova NV. Effect of metal ions and xenobioties on endogenous oxidation of DNA. Biochemistry ( Mosc ), 1997,62(1):88.
  • 4Saris CP, Damman SJ, van den Ende AM, et al.^32 P-postlabelling analysis of alkylphosphotriesters in DNA. IARC Sci Publ, 1993,124 :127.
  • 5Bonner AG,Udell LM ,Creaaey WA,et al. Solid -phase precipitation and extraction, a new separation process applied to the isolation of synthetic peptidea. J Pept Res,2001 ,57(1) :48.
  • 6Yin H, Racha J, Li SY, et al. Automated high throughput human CYP isoform activity assay using SPE - LC/MS method: application in CYP inhibition evaluation. Xenobioticu ,2000,30(2) : 141.
  • 7Homma M,Beckerman K, Hayashi S, et al. Liquid chromatographic determination of urinary 6beta - hydroxyeortisol to assess cytochrome P -450 3A activity in HIV positive pregnant women. J Pharm Biomed Anal,2000,23(4) :629.
  • 8Pascual JA, Sanagustin J. Fully automated analytical method for codeine quantification in human plasma using on - line solid - phase extraction and high - performance liquid chromatography with ultraviolet detection. J Chromatogr B Biomed Sci Appl, 1999 ,724 (2) :295.
  • 9Jemal M. High - throughput quantitative bioanalysis by LC/MS/MS. Biomed Chromutogr ,2000 ,14 (6) :422.
  • 10Ramis I, Hotter G, Rosello - Catafau J, et al. Application of totally automated on - line sample clean up system for extraction and high - performance liquid chromatography separation of peptide leukotrienes. J Pharm Biomed Anal,1993 ,1 ( 11 - 12) :1135.

共引文献17

同被引文献560

引证文献2

二级引证文献83

相关作者

内容加载中请稍等...

相关机构

内容加载中请稍等...

相关主题

内容加载中请稍等...

浏览历史

内容加载中请稍等...
;
使用帮助 返回顶部