- Title
- Method validation for the quantification of casticin in vitex agnus castus fruit using an ftir multivariate chemometric model
- Creator
- Du Toit Louw, Philippus
- Subject
- Drugs -- Analysis -- Methodology -- Evaluation
- Subject
- Alternative medicine -- Research
- Subject
- Liquid chromatography
- Date Issued
- 2018
- Date
- 2018
- Type
- Thesis
- Type
- Masters
- Type
- MPharm
- Identifier
- http://hdl.handle.net/10948/30917
- Identifier
- vital:31222
- Description
- The Complementary and Alternative Medicines (CAMS) and dietary supplement industry is an R8.84 billion a year industry in South Africa, with the sector expected to grow 12% annually. The industry has largely been unregulated up until 15 November 2013, when the South African government amended the Medicines and Related Substance Control Act (Act 101 of 1965) to include the definition of “Complementary Medicines” and “Health Supplements”. The emphasis of the new regulations is largely on the quality and safety of CAMS products. Manufacturers therefore need to demonstrate that the active ingredients used in manufacturing will be of an appropriate and consistent quality. The research question therefore is: Can a chemometric multivariate model be used to develop a rapid, cost effective method to quantify casticin, the major chemical constituent of Vitex agnus-castus (VAC) that can be used during routine quality control procedures? The primary aim of this study was to prepare a validated method using fourier transform infrared spectroscopy (FTIR) to quantify the casticin content in VAC fruit. The results from the HPLC analysis were as follows; the penduletin eluted at a retention time of 12.419 ± 0.376 minutes. The casticin eluted at a retention time of 12.943 ± 0.018 minutes. The casticin content for the samples ranged from 0.0115 – 0.0147% m/m casticin content with an average of 0.0134%. This is well below the pharmacopoeia requirement of not less than (NLT) 0.08% casticin content as described in the British Pharmacopoeia (BP). The results obtained from the HPLC analysis were used to construct the FTIR calibration model. The calibration model consisted of 18 spectra with 530 selected data points. The model was specific for casticin as spectral regions in the calibration model can be correlated to a known IR spectral response associated with the carbonyl group of casticin. The calibration equation in the xii form of % m/m casticin content had a coefficient of determination (R2) value of 0.9855 and a root mean square error of cross-validation (RMSECV) of 0.000119. The accuracy of the model had recoveries of between 98 - 102% for the actual vs true prediction. The percentage relative standard deviation (%RSD) between nine repeated measurements was 3.46%, this does not meet the International Conference of Harmonisation (ICH) requirement for precision of not more than (NMT) 2% RSD. The range of the calibration model was between 0.01147 and 0.01469 % m/m casticin content as established by the calibration model. The robustness of the method was assessed by challenging the model with samples that fall outside of the concentration of range of the model. This was established by quantifying previously scanned samples of VAC that is not part of the calibration set. The model was able to verify if the tested samples prediction was outside of the validated calibration range. The method was subsequently also challenged with a sample of a different identity to VAC. The model indicated that the sample tested does not fall in the range of the method and was clearly recognised as an outlier. The method was rapid and does not require any expensive solvents or timeconsuming sample preparation. However, the method does not meet the ICH requirements for method validation, the method does show potential and further method development and expansion of the calibration model can ensure that the method be validated.
- Format
- xiii, 75 leaves
- Format
- Publisher
- Nelson Mandela University
- Publisher
- Faculty of Health Sciences
- Language
- English
- Rights
- Nelson Mandela University
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| Thumbnail | File | Description | Size | Format | |||
|---|---|---|---|---|---|---|---|
| View Details Download | SOURCE1 | Philippus Du Toit Louw.pdf | 6 MB | Adobe Acrobat PDF | View Details Download |