Development and validation of a LC-MS/MS method for the determination of viaminate in human plasma.
A sensitive and specific method for determination of viaminate in human plasma by using high-performance liquid chromatography coupled with electrospray tandem mass spectrometry (LC-MS/MS) was developed in this study. The plasma samples were simply deproteinated, extracted, evaporated, and then reconstituted in 200 microl of methanol prior to analysis. Chromatographic separation was carried out on a Shimadzu VP-ODS column (250 mm x 2.0 mm, 5 microm) with a mobile phase of methanol-water (95:5, v/v) at a flow rate of 0.2 ml/min. Quantification was performed in the negative-ion electrospray ionization mode by selected ion monitoring of the product ions at m/z 164 for viaminate and m/z 109 for testosterone propionate which was used as the internal standard. The corresponding parent ions were m/z 446 and m/z 345. A linear calibration curve was observed within the concentration range of 0.10-200 ng/ml. The lowest limit of quantitation (LLOQ) was 0.1 ng/ml. The extraction-efficiency at three concentrations was 100.7, 93.6, and 99.7%. Practical utility of this new LC-MS/MS method was confirmed in pilot pharmacokinetic studies in humans following oral administration.
Yin
Jing
J
Department of Analytical Chemistry, China Pharmaceutical University, Nanjing 210009, China.
Ni
Kun-Yi
KY
Shen
Yue
Y
Ma
Peng-Cheng
PC
Cao
Ling
L
Wang
Wei-Peng
WP
Wang
Yu
Y
D002138:Calibration; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D006801:Humans; D012015:Reference Standards; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014212:Tretinoin / Q000031:analogs & derivatives* / Q000097:blood
C524512:viaminate; D014212:Tretinoin