Development and validation of an alternative titration method for the determination of sulfate ion in indinavir sulfate

Silva, Breno de Carvalho e; Campos, Lígia Maria Moreira de; Pianetti, Gérson Antônio

doi:10.1590/s0100-40422005000100011

Cited by 7 publications

(3 citation statements)

References 3 publications

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“…uses the determination of the sulfate ion as assay of the IDV drug substance. Silva et al14 described an alternative method for the estimation of the sulfate ion content. Lead nitrate was used instead of lead perchlorate as a titrant employing potentiometric determination using a lead‐specific electrode.…”

Section: Indinavirmentioning

confidence: 99%

Quality Control of Protease Inhibitors

Yekkala

Adams

Schepdael

et al. 2008

Journal of Pharmaceutical Sciences

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Section: Indinavirmentioning

confidence: 99%

Quality Control of Protease Inhibitors

Yekkala

Adams

Schepdael

et al. 2008

Journal of Pharmaceutical Sciences

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“…Indinavir lactone and cisamino-2-indanol can be formed due to amide hydrolysis [2][3][4][5]. Several methods have been described for the analysis of IDV, such as potentiometry [2,6,7], thin layer chromatography [2,6], capillary electrophoresis (CE) [3,[8][9][10][11], liquid chromatography (LC) with electrochemical detection [12], LC with UV detection * Corresponding author. Tel.…”

Section: Introductionmentioning

confidence: 99%

Evaluation of an International Pharmacopoeia method for the analysis of indinavir sulfate by liquid chromatography

Yekkala

Lei

Hoogmartens

et al. 2006

Journal of Pharmaceutical and Biomedical Analysis

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“…1 Indinavir is prescribed as a sulfate salt due to superior gastrointestinal solubility and absorption when compared with the free base. 2 When drugs are manufactured as salts, an analytical technique is required to confirm that correct levels of counter ion are present. 3 The counter ions of drugs with ionic groups are of importance because the physicochemical properties, stability and bioavailability of the drugs depend on their salt forms.…”

Section: Introductionmentioning

confidence: 99%

Development and validation of a capillary electrophoresis method for the determination of sulfate in indinavir sulfate raw material

Pereira¹,

Micke²,

Tavares³

2006

J. Braz. Chem. Soc.

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O presente trabalho descreve um método simples e rápido por eletroforese capilar, utilizando detecção indireta (230 nm) para determinação quantitativa de sulfato em sulfato de indinavir (matéria-prima). Uma solução contendo 10 mmol L -1 de molibdato de amônio e 0,15 mmol L -1 de brometo de cetiltrimetilamônio (pH 7,5) foi utilizada como eletrólito de corrida. As amostras foram injetadas hidrodinamicamente com pressão 5000 Pa durante 3 s. A resposta foi linear no intervalo entre 10,1 μg mL -1 a 79,8 μg mL -1 . Os limites de detecção e quantificação foram de 0,34 e 1,13 μg mL -1 , respectivamente. A precisão intra-dia, determinada como desvio padrão relativo, foi de 2,8% para dez preparações independentes da amostra. Os valores de recuperação para três diferentes níveis de concentração variaram de 96,9 a 102,4%. A metodologia foi aplicada a amostras reais. A concentração de sulfato na amostra variou de 13,3 a 13,5% (m/m, calculado com relação ao material seco).In this work, a simple and fast capillary electrophoresis method using indirect UV detection (230 nm) for the quantitative determination of sulfate in the indinavir sulfate raw material was described. A running electrolyte consisting of 10 mmol L -1 ammonium molybdate containing 0.15 mmol L -1 cetyltrimethylammonium bromide (pH 7.5) was used. Samples were injected hydrodynamically by applying 5000 Pa pressure during 3 s. The response was linear from 10.1 μg mL -1 to 79.8 μg mL -1 . Limits of detection and quantification were 0.34 and 1.13 μg mL -1 , respectively. The intra-day precision expressed as relative standard deviation was 2.8% for 10 independent sample preparations. Recoveries varying from 96.9 to 102.4% at three concentration levels were obtained. The methodology was successfully applied for real samples. The concentration of sulfate in indinavir sulfate raw material varied from 13.3 to 13.5% (m/m calculated as anhydrous base).Keywords: indinavir sulfate, capillary electrophoresis, sulfate, validation, HIV IntroductionIndinavir sulfate was approved by the FDA (Food and Drugs Administration) on March 13, 1996, for use in combination with other protease inhibitors, nucleoside analogues or reverse transcriptase inhibitors for the treatment against acquired immune deficiency syndrome (AIDS).1 Indinavir is prescribed as a sulfate salt due to superior gastrointestinal solubility and absorption when compared with the free base. When drugs are manufactured as salts, an analytical technique is required to confirm that correct levels of counter ion are present. 3 The counter ions of drugs with ionic groups are of importance because the physicochemical properties, stability and bioavailability of the drugs depend on their salt forms. An analytical technique such as ion chromatography (IC) and titrimetry is often used for the analysis of counter ion in pharmaceutical drug substances.3 However, these methods are laborious and time consuming, besides the high maintenance cost of IC technique.Capillary electrophoresis (CE) has been successfully applied to the ana...

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Development and validation of an alternative titration method for the determination of sulfate ion in indinavir sulfate

Cited by 7 publications

References 3 publications

Quality Control of Protease Inhibitors

Quality Control of Protease Inhibitors

Evaluation of an International Pharmacopoeia method for the analysis of indinavir sulfate by liquid chromatography

Development and validation of a capillary electrophoresis method for the determination of sulfate in indinavir sulfate raw material

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