Quantitative determination of the polypeptide motilin in rat plasma by externally calibrated liquid chromatography/electrospray ionization mass spectrometry

被引:21
作者
Delinsky, DC [1 ]
Hill, KT [1 ]
White, CA [1 ]
Bartlett, MG [1 ]
机构
[1] Univ Georgia, Dept Pharmaceut & Biomed Sci, Coll Pharm, Athens, GA 30602 USA
关键词
D O I
10.1002/rcm.1328
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
We present a method for the quantitation of motilin from rat plasma by protein precipitation and liquid chromatography/mass spectrometry (LC/MS). Using external calibration, the method was linear over the concentration range 10-1000 ng/mL with an initial sample volume of 150 muL. The LC system included a C-18 column with a 300 Angstrom pore size. A linear gradient was used with a mobile phase consisting of water and acetonitrile, each with 0.2% acetic acid and 0.02% trifluoroacetic acid. Motilin was detected with the mass spectrometer in positive ion mode monitoring the 4+ charge state at m/z 675.5. The approximated limit of detection was less than 1 ng/mL and the lower limit of quantitation (LLOQ) was 10 ng/mL. The method showed a high degree of precision and accuracy both within and between runs at five validation points, including the LLOQ. Copyright (C) 2004 John Wiley Sons, Ltd.
引用
收藏
页码:293 / 298
页数:6
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