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

Megoulas, Nikolaos C.; Koupparis, Michael A.

doi:10.1016/j.jpba.2004.05.018

Cited by 70 publications

(40 citation statements)

References 19 publications

Supporting

Mentioning

Contrasting

Unclassified

Order By: Relevance

“…Gentamicin has an important potential use against a wide spectrum of Gram-negative and Gram-positive bacteria, however, many of its applications are restricted to low dose administrations, mainly because of the appearance of residues in the kidney and the high cost of the treatment (1). It is administrated in the form of injection, cream, ointment, suspension and it is also used in veterinary medicine (2).…”

Section: Introductionmentioning

confidence: 99%

Niosome-Encapsulated Gentamicin for Ophthalmic Controlled Delivery

2008

View full text Add to dashboard Cite

Abstract. The objective of the present research was to investigate the feasibility of using non-ionic surfactant vesicles (niosomes) as carriers for the ophthalmic controlled delivery of a water soluble local antibiotic; gentamicin sulphate. Niosomal formulations were prepared using various surfactants (Tween 60, Tween 80 or Brij 35), in the presence of cholesterol and a negative charge inducer dicetyl phosphate (DCP) in different molar ratios and by employing a thin film hydration technique. The ability of these vesicles to entrap the studied drug was evaluated by determining the entrapment efficiency %EE after centrifugation and separation of the formed vesicles. Photomicroscopy and transmission electron microscopy as well as particle size analysis were used to study the formation, morphology and size of the drug loaded niosomes. Results showed a substantial change in the release rate and an alteration in the %EE of gentamicin sulphate from niosomal formulations upon varying type of surfactant, cholesterol content and presence or absence of DCP. In-vitro drug release results confirmed that niosomal formulations have exhibited a high retention of gentamicin sulphate inside the vesicles such that their in vitro release was slower compared to the drug solution. A preparation with 1:1:0.1 molar ratio of Tween 60, cholesterol and DCP gave the most advantageous entrapment (92.02%±1.43) and release results (Q 8h =66.29%±1.33) as compared to other compositions. Ocular irritancy test performed on albino rabbits, showed no sign of irritation for all tested niosomal formulations.

show abstract

Section: Introductionmentioning

confidence: 99%

Niosome-Encapsulated Gentamicin for Ophthalmic Controlled Delivery

2008

View full text Add to dashboard Cite

show abstract

“…High-performance liquid chromatography coupled with evaporative light scattering detection (HPLC-ELSD) has been used for the analysis of many non-UV-absorbing analytes [22][23][24][25][26][27][28]. Several HPLC-ELSD methods have been developed to determine spectinomycin and its related substances [6,7,29].…”

Section: Introductionmentioning

confidence: 99%

“…There are limited reports of AG separation in normal-phase mode, but these may result in the loss of column materials. Therefore, most chromatographic methods were based on ion-pairing reversed-phase system, which should be volatile when combined with ELSD [24,27]. Similar to mass spectrometry (MS), ELSD separation products are easily transferred to collect structural information of minor impurities in pharmaceutical products [30][31][32][33][34].…”

Section: Introductionmentioning

confidence: 99%

Determination of spectinomycin and related substances by HPLC coupled with evaporative light scattering detection

Wang¹,

Wang²,

Li³

et al. 2015

Acta Chromatographica

View full text Add to dashboard Cite

Summary. An improved ion-pairing reversed-phase high-performance liquid chromatography method coupled with evaporative light scattering detection (HPLC-ELSD) was developed to determine spectinomycin and its related substances in commercial samples. The method was validated in accordance with International Conference on Harmonization (ICH) guidelines. The specificity of the HPLC-ELSD method was similar to that of the European Pharmacopoeia (Ph. Eur.) method, and repeatability and robustness were markedly improved relative to other reported methods due to our empirical evaluation of separation columns. Indeed, it is a more specific assay of spectinomycin than traditional microbiological techniques. The HPLC-ELSD method was used to evaluate the impurity profiles of eight compounds in seven spectinomycin batches from five different companies. Liquid chromatography coupled with electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) was employed to characterize the structures of these compounds. Though the HPLC-ELSD method was not as sensitive as the Ph. Eur. method, its limit of quantitation (LOQ) (0.16%) was lower than the disregard limit (0.3%) described by the Ph. Eur. 7.0. This suggests that the HPLC-ELSD method is appropriate for routine analysis of spectinomycin and its related substances.

show abstract

“…While this method has several benefits, there are also some limitations such as low selectivity, requirement for volatile mobile phase, nonlinear response, and also being destructive to the sample (25). This detection method has been applied effectively for at least the last two decades to quantify a wide spectrum of natural and synthetic compounds including pharmaceuticals (i.e., drug molecules and excipients including polymers, sugars, lipids, and surfactants) (4,24,(26)(27)(28)(29), natural products and biologics (30,31). foods, and beverages (32,33).…”

Section: Introductionmentioning

confidence: 99%

Development of a Robust Method for Simultaneous Quantification of Polymer (HPMC) and Surfactant (Dodecyl β-D-Maltoside) in Nanosuspensions

Patel

Bummer

2015

AAPS PharmSciTech

View full text Add to dashboard Cite

Abstract. This report describes the development of a chromatographic method for the simultaneous quantification of a polymer, hydroxypropyl methylcellulose (HPMC), and a surfactant, dodecyl β-Dmaltoside (DM), that are commonly used in the physical stabilization of pharmaceutical formulations such as nanosuspensions and solid dispersions. These excipients are often challenging to quantify due to the lack of chromophores. A reverse phase size exclusion chromatography (SEC) with evaporative light scattering detector (ELSD) technique was utilized to develop an accurate and robust assay for the simultaneous quantification of HPMC and DM in a nanosuspension formulation. The statistical design of experiments was used to determine the influence of critical ELSD variables including temperature, pressure, and gain on accuracy, precision, and sensitivity of the assay. A robust design space was identified where it was determined that an increase in the temperature of the drift tube and gain of the instrument increased the accuracy and precision of the assay and a decrease in the nebulizer pressure value increased the sensitivity of the assay. In the optimized design space, response data showed that the assay could quantify HPMC and DM simultaneously with good accuracy, precision, and reproducibility. Overall, SEC-ELSD proved to be a powerful technique for the simultaneous quantification of HPMC and DM. This technique can be used to quantify the amount of HPMC and DM in nanosuspensions, which is critical to understanding their effects on the physical stability of nanosuspensions.KEY WORDS: design of experiments; dodecyl β-D-maltoside; evaporative light scattering detector; HPMC; nanosuspensions.

show abstract

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

Cited by 70 publications

References 19 publications

Niosome-Encapsulated Gentamicin for Ophthalmic Controlled Delivery

Niosome-Encapsulated Gentamicin for Ophthalmic Controlled Delivery

Determination of spectinomycin and related substances by HPLC coupled with evaporative light scattering detection

Development of a Robust Method for Simultaneous Quantification of Polymer (HPMC) and Surfactant (Dodecyl β-D-Maltoside) in Nanosuspensions

Contact Info

Product

Resources

About