Development and validation of a novel LC/ELSD method for the quantitation of gentamicin sulfate components in pharmaceuticals.

Abstract:

:The equivalent response of evaporative light scattering detector (ELSD) for compounds of similar structure is exploited to develop an LC/ELSD method for the simultaneous quantitation of the four main components of gentamicin sulfate, using as external standard the one main component kanamycin. A C18 column was used along with a mobile phase consisting of H2O (containing 35.4 microg/ml of trichloroacetic acid and 0.89 microl/ml of trifluoroacetic acid)-methanol-acetonitrile (990:5:5, v/v/v), in an isocratic mode at 1.1 ml/min. Parameters of ELSD were 50 degrees C for evaporation temperature and 3.0 bar for pressure of carrier gas (N2). A logarithmic calibration curve was obtained for sulfate (tR = 1.9 min) from 4.2 to 150 microg/ml (r > 0.994) with a precision of 0.18%R.S.D. Kanamycin and the four gentamicin components (C(1a), C2, C(2a) and C1) were eluted at 3.2, 4.6, 5.9, 7.1 and 8.7 min, respectively, with good resolution (Rs > 1.5). Logarithmic calibration curve was obtained for each component (r > 0.99) with statistically equal slopes varying from 2.457 to 2.558. The mass range of total gentamycin was 35-240 microg/ml. The proposed method was applied for the determination of gentamicin components and sulfate in raw materials and pharmaceutical formulations (injection, drops and cream) without any pretreatment except cream, for which liquid-liquid extraction was required. Recovery from standard addition experiments in commercial formulations was 99-100% regarding total gentamicin and 89-108% regarding individual components, with a precision (%RSD, n = 4) 0.7-5.8%.

journal_name

J Pharm Biomed Anal

authors

Megoulas NC,Koupparis MA

doi

10.1016/j.jpba.2004.05.018

subject

Has Abstract

pub_date

2004-09-21 00:00:00

pages

73-9

issue

1

eissn

0731-7085

issn

1873-264X

pii

S0731708504002468

journal_volume

36

pub_type

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