摘要
目的建立液-质联用(HPLC-MS)测定人血浆中地塞米松浓度的方法。方法采用Agilent Zorbax Extend C18色谱柱(2.1mm×150 mm,5μm),以0.4%醋酸铵溶液-乙腈(62:38)为流动相,流速0.25 mL·min-1,在血浆中加入内标醋酸泼尼松,固相萃取后采用HPLC-MS(ESI源)测定地塞米松的血浆浓度。结果地塞米松在人血浆中0.02~4 mg·L-1内线性良好,最低检测限为0.02 mg·L-1,绝对回收率>95%,相对回收率在98.84%~102.80%之间,日内及日间RSD均小于3%。结论本方法能满足人血浆中地塞米松浓度的测定。
Abstract
OBJECTIVE To develop and validate a HPLC-MS method for determining dexamethasone in human plasma.METHODS The separation was performed on a column of Zorbax Extend C18(2.1mm×150 mm,5 μm). The mobile phase consisted of 0.4% ammonium acetate solution-acetonitrile(62-38) .Using solid phase extraction, dexamethasone in human plasma was measured by HPLC-MS with ESI. The internal standard was prednisone acetate.RESULTS The standard curve was linear over the range of 0.02~4 mg·L-1. The lowest dexamethasone concentration that gave a reproducible integration was 0.02 mg·L-1.The absolute recovery was more than 95%,the relative recovery was among the range of 98.84%~102.80%.The RSDs of intra-day and inter-day validation were less than 3% . CONCLUSION HPLC-MS may be used for the determination of dexamethasone in human plasma.
关键词
地塞米松 /
高效液相色谱-质谱 /
血药浓度
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Key words
dexamethasone /
HPLC-MS /
concentration
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刘蕾;付逸龙;殷琦;李可欣;孙春华.
SPE-HPLC-MS测定人血浆中地塞米松浓度[J]. 中国药学杂志, 2005, 39(09): 705-707
LIU Lei;FU Yi-long;YIN Qi;LI Ke-xin;SUN Chun-hu.
Determination of dexamethasone in human plasma by SPE-HPLC-MS [J]. Chinese Pharmaceutical Journal, 2005, 39(09): 705-707
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参考文献
[1]Toth GG, Kloosterman C, Uges DR,et al. Pharmacokinetics of high-dose oral and intravenous dexamethasone[J].Ther Drug Monit,1999,21(5):532.
[2]Ifa DR, Moraes ME, Moraes MO,et al. Determination of 21-hydroxydeflazacort in human plasma by high-performance liquid chromatography/atmospheric pressure chemical ionization tandem mass spectrometry. Application to bioequivalence study[J].J Mass Spectrom,2000,35(3):440.
[3]Garcia CV, Breier AR, Steppe M,et al. Determination of dexamethasone acetate in cream by HPLC[J].J Pharm Biomed Anal,2003,31(3):597.
[4]Lemus GJM, Perez AJ. Simultaneous determination of dexamethasone and trimethoprim by liquid chromatography[J].J Pharm Biomed Anal,2002,30(4):1255.
[5]Stolke AAM, Schwillens PLWJ, van Ginkel LA, et al. Comparison of different liquid chromatography methods for the determination of corticosteroids in biological matrices[J].J Chromatogr A,2000,893(1):55.
[6]Paul NS, Bruce GC. Determination of dexamethasone in plasma of premature neonates using high-performance liquid chromatography[J].J Chromatogr B,1994,658(2):189.
[7]Noben JP, Gielen B, Royackers E,et al. A high-performance liquid chromatography/tandem mass spectrometric screening method for eight synthetic corticosteroids in bovine feces and the simultaneous differentiation between dexamethasone and betamethasone[J].Rapid Commun Mass Spectrom,2002,16(16):1590.
[8]Wasch KF, Brabander D, Wiele M,et al. Differentiation between dexamethasone and betamethasone in a mixture using multiple mass spectrometry[J].J Chromatogr A,2001,926(4):79.
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脚注
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