Published:Journal of Chromatographic Science,
ISSN 0021-9665 Volume 45,
Number 3, March 2007, pp.126-130
Analysis of Monoethanolamine by Derivatization
with Marfey’s Reagent and HPLC
Kenley K. Ngim[1], Jacob Zynger[1], and Brian
Downey[2]
[1]Aptuit, Inc., 10245 Hickman Mills Drive, Kansas City, MO 64137
and
[2]POZEN Inc., 1414 Raleigh Road, Suite 400, Chapel Hill, NC 27517
A sensitive and selective method for determining
the residual monoethanolamine in a developmental drug substance
is developed and validated. Marfey’s reagent, which is commonly
used for the chiral analysis of amino acids, is reacted with the
primary amine group of monoethanolamine and then analyzed by high-performance
liquid chromatography–UV at 340 nm. Quantitation is performed
by a standard addition method by preparing drug substance samples
with added monoethanolamine ranging from 0.25–1.0 µg/mL
(equivalent to 12.5–50 ppm with respect to the drug substance).
The method performance is evaluated for linearity, specificity,
detection and quantitation limits, accuracy, precision, and sample
stability. The method is linear from 0.25–1.0 µg/mL
with a coefficient of determination (r2) > 0.95. The accuracy
and precision obtained is 105.5 ± 4.8% (n = 3). The limits
of detection and quantitation are 0.03 and 0.10 µg/mL, respectively.
Instrument precision (% relative standard deviation of six injections
of a derivatized 0.5 µg/mL monoethanolamine solution on
two separate days) is ≥ 2.0%. This method is suitable for
the determination of monoethanolamine at the 25 ppm level in drug
substance.
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