The Quality of Antimalarials - A Study in Selected African Countries - EDM Research Series No. 030
(2003; 67 pages) View the PDF document
Table of Contents
View the documentAuthors
View the documentCountry Research Team Leaders
View the documentLaboratory Support
View the documentAcknowledgements
View the documentAcronyms
View the documentExecutive summary
View the document1. Background
Close this folder2. Methodology
Close this folder2.1 Analytical methods
View the document2.1.1 Method for the assay of chloroquine syrup
View the document2.1.2 Method for the assay of chloroquine tablets
View the document2.1.3 Method for the assay of sulphadoxine/pyrimethamine tablets
Open this folder and view contents2.2 Dissolution testing
View the document3. Results
Open this folder and view contents4. Discussion
Open this folder and view contents5. Conclusions and recommendations
View the documentReferences
Open this folder and view contentsTables
Open this folder and view contentsAnnexes
View the documentOther documents in the EDM Research Series
View the documentEDM Research Series No. 30
 

2.1.1 Method for the assay of chloroquine syrup

There is no analytical monograph in the United States Pharmacopeia (USP) or British Pharmacopoeia (BP) for the assay of chloroquine syrup. A high pressure liquid chromatography (HPLC) method was developed and validated in-house for the determination of chloroquine in chloroquine syrup. Validation of the method was carried out according to the validation criteria of the USP and the guidelines of the International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use. Validation parameters, such as specificity, linearity, accuracy and precision, as well as chromatographic parameters, such as peak symmetry and resolution, were assessed and optimized.

As the laboratory did not know the type of excipients used in the various formulations, the method was only validated for interference from the most generally used preservatives such as the parabens (hydroxy benzoates) and benzoic acid. Evidence of interference from any other preservative not validated for could not be detected during the analysis, and therefore the HPLC method was assumed to be specific for the determination of chloroquine in chloroquine syrup.

The method parameters were as follows:

HPLC column:

C18, 150 x 4.6 mm

Mobile phase:

75% 0.1M KH2PO4: 25% acetonitrile, 200mg heptane sulfonic acid (pH 3.5)

Detection:

UV at 330 nm

Flow rate:

2ml/min

Injection volume:

20 µl

Performance criteria of the method:

Specificity:

Specific for chloroquine in the presence of hydroxy benzoates and benzoic acid

Precision:

%RSD < 2.0

Linearity:

> 0.98.

Symmetry:

<1.5

Although the method was not specifically validated to indicate all five possible decomposition products due to photo degradation, no peaks suggesting the decomposition of the analyte before or during the analyses were observed.

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