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Published:Journal of Chromatographic Science,
ISSN 0021-9665Volume 44,
Number 9, October 2006, pp.529-534
Determination
of Vertilmicin Sulfate and Its Related Substances by HPLC–ELSD
and HPLC–MS2
Jian Wang, Dandan Wang, Hua He, and Kunyi Ni
Department of Analytical Chemistry, China Pharmaceutical University, No. 24,
Nanjing, 210009, China
A new and simple high-performance liquid
chromatography (HPLC)–evaporative light scattering detection
(ELSD) method for the determination of vertilmicin sulfate
and its related substances is developed. The column is an Agilent
SB-C18 (250 ¥ 4.6 mm, 5 µm). The mobile phase is
0.05 mol/L trifluoroacetic acid–methanol (85:15). Good
separation of vertilmicin from the main related substances
is achieved. The standard curve is rectilinear in the range
of 270–1350 µg/mL (r = 0.9998). The average recovery
is 99.8%. The limit of detection is 10 µg/mL. The HPLC–mass
spectrometry–mass spectrometry (MS2) method is used to
characterize the structures of vertilmicin sulfate and its
related substances. In positive mode, vertilmicin sulfate and
its related substances are elucidated by use of electrospray
ion trap MS in the multi-stage MS full scan mode. The possible
structure of an unknown impurity in vertilmicin is deduced
based on the HPLC–MS2 data.
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