A stability-indicating high performance liquid chromatographic assay for the determination of orlistat in capsules
- Mohammadi, Ali, Haririan, I, Rezanour, I, Ghiasi, L, Walker, Roderick B
- Authors: Mohammadi, Ali , Haririan, I , Rezanour, I , Ghiasi, L , Walker, Roderick B
- Date: 2006
- Language: English
- Type: Article , text
- Identifier: vital:6407 , http://hdl.handle.net/10962/d1006480
- Description: A stability-indicating HPLC method was developed and validated for the quantitative determination of orlistat in capsule dosage forms. An isocratic separation was achieved using a Perfectsil® target ODS-3, 250 mm × 4.6 mm i.d., 5 µm particle size column with a flow rate of 0.7 ml/min and using a UV detector to monitor the eluate at 210 nm. The mobile phase consisted of methanol:acetonitrile:trifluoroacetic acid (82.5:17.5:0.01, v/v/v). The drug was subjected oxidation, hydrolysis, photolysis and heat to apply stress conditions. Complete separation was achieved for the parent compound and all degradation products in an overall analytical run time of approximately 15 min with the parent compound orlistat eluting at approximately 9 min. The method was linear over the concentration range of 0.02–0.75 mg/ml (r = 0.9998) with a limit of detection and quantitation 0.006 and 0.02 mg/ml, respectively. The method has the requisite accuracy, selectivity, sensitivity and precision to assay orlistat in capsules. Degradation products resulting from the stress studies did not interfere with the detection of orlistat and the assay is thus stability-indicating.
- Full Text:
- Authors: Mohammadi, Ali , Haririan, I , Rezanour, I , Ghiasi, L , Walker, Roderick B
- Date: 2006
- Language: English
- Type: Article , text
- Identifier: vital:6407 , http://hdl.handle.net/10962/d1006480
- Description: A stability-indicating HPLC method was developed and validated for the quantitative determination of orlistat in capsule dosage forms. An isocratic separation was achieved using a Perfectsil® target ODS-3, 250 mm × 4.6 mm i.d., 5 µm particle size column with a flow rate of 0.7 ml/min and using a UV detector to monitor the eluate at 210 nm. The mobile phase consisted of methanol:acetonitrile:trifluoroacetic acid (82.5:17.5:0.01, v/v/v). The drug was subjected oxidation, hydrolysis, photolysis and heat to apply stress conditions. Complete separation was achieved for the parent compound and all degradation products in an overall analytical run time of approximately 15 min with the parent compound orlistat eluting at approximately 9 min. The method was linear over the concentration range of 0.02–0.75 mg/ml (r = 0.9998) with a limit of detection and quantitation 0.006 and 0.02 mg/ml, respectively. The method has the requisite accuracy, selectivity, sensitivity and precision to assay orlistat in capsules. Degradation products resulting from the stress studies did not interfere with the detection of orlistat and the assay is thus stability-indicating.
- Full Text:
A stability-indicating high performance liquid chromatographic assay for the determination of orlistat in capsules
- Mohammadi, Ali, Haririan, I, Rezanour, Nasrin, Ghiasi, L, Walker, Roderick B
- Authors: Mohammadi, Ali , Haririan, I , Rezanour, Nasrin , Ghiasi, L , Walker, Roderick B
- Date: 2006
- Subjects: To be catalogued
- Language: English
- Type: text , article
- Identifier: http://hdl.handle.net/10962/184267 , vital:44195 , xlink:href="https://doi.org/10.1016/j.chroma.2006.03.038"
- Description: A stability-indicating HPLC method was developed and validated for the quantitative determination of orlistat in capsule dosage forms. An isocratic separation was achieved using a Perfectsil® target ODS-3, 250 mm × 4.6 mm i.d., 5 μm particle size column with a flow rate of 0.7 ml/min and using a UV detector to monitor the eluate at 210 nm. The mobile phase consisted of methanol:acetonitrile:trifluoroacetic acid (82.5:17.5:0.01, v/v/v). The drug was subjected oxidation, hydrolysis, photolysis and heat to apply stress conditions. Complete separation was achieved for the parent compound and all degradation products in an overall analytical run time of approximately 15 min with the parent compound orlistat eluting at approximately 9 min. The method was linear over the concentration range of 0.02–0.75 mg/ml (r = 0.9998) with a limit of detection and quantitation 0.006 and 0.02 mg/ml, respectively. The method has the requisite accuracy, selectivity, sensitivity and precision to assay orlistat in capsules. Degradation products resulting from the stress studies did not interfere with the detection of orlistat and the assay is thus stability-indicating.
- Full Text:
- Authors: Mohammadi, Ali , Haririan, I , Rezanour, Nasrin , Ghiasi, L , Walker, Roderick B
- Date: 2006
- Subjects: To be catalogued
- Language: English
- Type: text , article
- Identifier: http://hdl.handle.net/10962/184267 , vital:44195 , xlink:href="https://doi.org/10.1016/j.chroma.2006.03.038"
- Description: A stability-indicating HPLC method was developed and validated for the quantitative determination of orlistat in capsule dosage forms. An isocratic separation was achieved using a Perfectsil® target ODS-3, 250 mm × 4.6 mm i.d., 5 μm particle size column with a flow rate of 0.7 ml/min and using a UV detector to monitor the eluate at 210 nm. The mobile phase consisted of methanol:acetonitrile:trifluoroacetic acid (82.5:17.5:0.01, v/v/v). The drug was subjected oxidation, hydrolysis, photolysis and heat to apply stress conditions. Complete separation was achieved for the parent compound and all degradation products in an overall analytical run time of approximately 15 min with the parent compound orlistat eluting at approximately 9 min. The method was linear over the concentration range of 0.02–0.75 mg/ml (r = 0.9998) with a limit of detection and quantitation 0.006 and 0.02 mg/ml, respectively. The method has the requisite accuracy, selectivity, sensitivity and precision to assay orlistat in capsules. Degradation products resulting from the stress studies did not interfere with the detection of orlistat and the assay is thus stability-indicating.
- Full Text:
Bioequivalence assessment of generic products an innovative South African approach
- Walker, Roderick B, Kanfer, Isadore, Skinner, Michael F
- Authors: Walker, Roderick B , Kanfer, Isadore , Skinner, Michael F
- Date: 2006
- Subjects: To be catalogued
- Language: English
- Type: text , article
- Identifier: http://hdl.handle.net/10962/184256 , vital:44194 , xlink:href="https://doi.org/10.1080/10601330500534014"
- Description: Concurrent with the implementation of new legislation mandating Generic Substitution in South Africa, a new set of guidelines for bioavailability and bioequivalence have been published. Since one of the main objectives of the new legislation in South Africa relating to Generic Substitution is to ensure that medicines of high quality, safety, and efficacy are made more accessible and more affordable to the wider public, the need to speed up approval of such multi-source products has become a regulatory priority. In order to facilitate this process, various bioequivalence issues have been addressed including important issues such as the acceptance criteria and associated bioequivalence intervals, use of a foreign reference product and the issue of assessing highly variable drugs (HVDs). In addition, dispensations have been made with respect to food effect assessment and variability relating to genetic polymorphism in drug metabolism (genotyping/phenotyping). Furthermore, the use of “old” biostudies submitted in support of an application is subject to expiry date. Acceptance of appropriate data requires that specific criteria such as Cmax and AUC, in addition to the usual considerations, also meet the limits specified by the particular registration authority of the country where such products are intended to be marketed. Generally, these limits require that the 90% confidence interval (CI) for AUC and Cmax test/reference ratios lies within the acceptance interval of 0.80–1.25 calculated using log-transformed data. While such acceptance criteria are, in general, ubiquitous, some differences in acceptance criteria do exist between various countries. The new guidelines for bioavailability/bioequivalence studies developed by the South African regulatory authority, the Medicines Control Council (MCC), makes provision for highly variable drugs and the use of a non-South African reference product. The MCC requires that the acceptance criterion for Cmax ratios be set at 0.75–1.33 while maintaining AUC ratios at 0.80–1.25 using a 90% CI. Furthermore, provision is made to apply scaling based on average bioequivalence assessment and, as an interim measure, consideration has also been given to the use of a foreign reference product provided that equivalence between that product and the innovator product currently available on the South African market can be shown using in vitro testing.
- Full Text:
- Authors: Walker, Roderick B , Kanfer, Isadore , Skinner, Michael F
- Date: 2006
- Subjects: To be catalogued
- Language: English
- Type: text , article
- Identifier: http://hdl.handle.net/10962/184256 , vital:44194 , xlink:href="https://doi.org/10.1080/10601330500534014"
- Description: Concurrent with the implementation of new legislation mandating Generic Substitution in South Africa, a new set of guidelines for bioavailability and bioequivalence have been published. Since one of the main objectives of the new legislation in South Africa relating to Generic Substitution is to ensure that medicines of high quality, safety, and efficacy are made more accessible and more affordable to the wider public, the need to speed up approval of such multi-source products has become a regulatory priority. In order to facilitate this process, various bioequivalence issues have been addressed including important issues such as the acceptance criteria and associated bioequivalence intervals, use of a foreign reference product and the issue of assessing highly variable drugs (HVDs). In addition, dispensations have been made with respect to food effect assessment and variability relating to genetic polymorphism in drug metabolism (genotyping/phenotyping). Furthermore, the use of “old” biostudies submitted in support of an application is subject to expiry date. Acceptance of appropriate data requires that specific criteria such as Cmax and AUC, in addition to the usual considerations, also meet the limits specified by the particular registration authority of the country where such products are intended to be marketed. Generally, these limits require that the 90% confidence interval (CI) for AUC and Cmax test/reference ratios lies within the acceptance interval of 0.80–1.25 calculated using log-transformed data. While such acceptance criteria are, in general, ubiquitous, some differences in acceptance criteria do exist between various countries. The new guidelines for bioavailability/bioequivalence studies developed by the South African regulatory authority, the Medicines Control Council (MCC), makes provision for highly variable drugs and the use of a non-South African reference product. The MCC requires that the acceptance criterion for Cmax ratios be set at 0.75–1.33 while maintaining AUC ratios at 0.80–1.25 using a 90% CI. Furthermore, provision is made to apply scaling based on average bioequivalence assessment and, as an interim measure, consideration has also been given to the use of a foreign reference product provided that equivalence between that product and the innovator product currently available on the South African market can be shown using in vitro testing.
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Development and validation of a stability-indicating analytical method for the quantitation of oxytocin in pharmaceutical dosage forms
- Chaibva, Faith A, Walker, Roderick B
- Authors: Chaibva, Faith A , Walker, Roderick B
- Date: 2006
- Language: English
- Type: Article
- Identifier: vital:6349 , http://hdl.handle.net/10962/d1006030
- Description: A single stability-indicating assay for oxytocin (OT) in pharmaceutical dosage forms using gradient elution over 21 min has been reported in the literature. Furthermore, published and compendial methods for the analysis of OT containing dosage forms also involve using HPLC with gradient elution and complicated mobile phases that include hydrophobic ion pairing agents. A simple isocratic and stability-indicating assay was developed and validated. The conditions are as follows, column: Phenomenex® C18 Hypersil, 5 μm packing, 4.6 mm × 150 mm with acetonitrile–phosphate buffer (pH 5; 0.08 M) (20:80) as the mobile phase with UV detection at 220 nm The method was found to be specific for OT in the presence of degradation products and chlorbutol (preservative) with an overall analytical run time of 16 min. Accuracy was determined to be 0.77–1.18% bias for all samples tested. Intra-assay precision (repeatability) was found to be 0.22–1.04%R.S.D. while the inter-day precision (intermediate precision) was found to be 1.27–1.68%R.S.D. for the samples studied. The calibration curve was found to be linear with the equation y = 1.81x + 0.02 and a linear regression coefficient of 0.9991 over the range 0.4–12.0 IU/ml. The LOD and the LOQ were determined to be 0.1 and 0.4 IU/ml, respectively. Syntocinon®, a commercially available dosage form of OT was assayed resulting in 100.5–106.6% recovery of the label claim and an average of 10.04 IU/ml.
- Full Text:
- Authors: Chaibva, Faith A , Walker, Roderick B
- Date: 2006
- Language: English
- Type: Article
- Identifier: vital:6349 , http://hdl.handle.net/10962/d1006030
- Description: A single stability-indicating assay for oxytocin (OT) in pharmaceutical dosage forms using gradient elution over 21 min has been reported in the literature. Furthermore, published and compendial methods for the analysis of OT containing dosage forms also involve using HPLC with gradient elution and complicated mobile phases that include hydrophobic ion pairing agents. A simple isocratic and stability-indicating assay was developed and validated. The conditions are as follows, column: Phenomenex® C18 Hypersil, 5 μm packing, 4.6 mm × 150 mm with acetonitrile–phosphate buffer (pH 5; 0.08 M) (20:80) as the mobile phase with UV detection at 220 nm The method was found to be specific for OT in the presence of degradation products and chlorbutol (preservative) with an overall analytical run time of 16 min. Accuracy was determined to be 0.77–1.18% bias for all samples tested. Intra-assay precision (repeatability) was found to be 0.22–1.04%R.S.D. while the inter-day precision (intermediate precision) was found to be 1.27–1.68%R.S.D. for the samples studied. The calibration curve was found to be linear with the equation y = 1.81x + 0.02 and a linear regression coefficient of 0.9991 over the range 0.4–12.0 IU/ml. The LOD and the LOQ were determined to be 0.1 and 0.4 IU/ml, respectively. Syntocinon®, a commercially available dosage form of OT was assayed resulting in 100.5–106.6% recovery of the label claim and an average of 10.04 IU/ml.
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Evaluation of rate of swelling and erosion of verapamil (VRP) sustained-release matrix tablets
- Khamanga, Sandile M, Walker, Roderick B
- Authors: Khamanga, Sandile M , Walker, Roderick B
- Date: 2006
- Subjects: To be catalogued
- Language: English
- Type: text , article
- Identifier: http://hdl.handle.net/10962/184232 , vital:44192 , xlink:href="https://doi.org/10.1080/03639040600599822"
- Description: Tablets manufactured in-house were compared to a marketed sustained-release product of verapamil to investigate the rate of hydration, erosion, and drug-release mechanism by measuring the wet and subsequent dry weights of the products. Swelling and erosion rates depended on the polymer and granulating fluid used, which ultimately pointed to their permeability characteristics. Erosion rate of the marketed product was highest, which suggests that the gel layer that formed around these tablets was weak as opposed to the robust and resistant layers of test products. Anomalous and near zero-order transport mechanisms were dominant in tests and commercial product, respectively.
- Full Text:
- Authors: Khamanga, Sandile M , Walker, Roderick B
- Date: 2006
- Subjects: To be catalogued
- Language: English
- Type: text , article
- Identifier: http://hdl.handle.net/10962/184232 , vital:44192 , xlink:href="https://doi.org/10.1080/03639040600599822"
- Description: Tablets manufactured in-house were compared to a marketed sustained-release product of verapamil to investigate the rate of hydration, erosion, and drug-release mechanism by measuring the wet and subsequent dry weights of the products. Swelling and erosion rates depended on the polymer and granulating fluid used, which ultimately pointed to their permeability characteristics. Erosion rate of the marketed product was highest, which suggests that the gel layer that formed around these tablets was weak as opposed to the robust and resistant layers of test products. Anomalous and near zero-order transport mechanisms were dominant in tests and commercial product, respectively.
- Full Text:
Generic substitution: the use of medicinal products containing different salts and implications for safety and efficacy
- Verbeeck, R K, Kanfer, Isadore, Walker, Roderick B
- Authors: Verbeeck, R K , Kanfer, Isadore , Walker, Roderick B
- Date: 2006
- Language: English
- Type: text , Article
- Identifier: vital:6445 , http://hdl.handle.net/10962/d1006632
- Description: In their quest to gain early entry of new generic products into the market prior to patent expiration, one of the strategies pursued by generic drug product manufacturers is to incorporate different salts of an approved active pharmaceutical ingredient (API) in a brand company's marketed dosage form and subject such dosage forms to bioequivalence assessment. These initiatives present challenges to regulatory authorities where the decision to approve bioequivalent products containing such pharmaceutical alternatives must be considered in the light of safety and efficacy, and more particularly, with respect to their substitutability. This article describes the various issues and contentions associated with the concept of pharmaceutical alternatives, specifically with respect to the uses of different salts and the implications for safety, efficacy and generic substitution.
- Full Text:
- Authors: Verbeeck, R K , Kanfer, Isadore , Walker, Roderick B
- Date: 2006
- Language: English
- Type: text , Article
- Identifier: vital:6445 , http://hdl.handle.net/10962/d1006632
- Description: In their quest to gain early entry of new generic products into the market prior to patent expiration, one of the strategies pursued by generic drug product manufacturers is to incorporate different salts of an approved active pharmaceutical ingredient (API) in a brand company's marketed dosage form and subject such dosage forms to bioequivalence assessment. These initiatives present challenges to regulatory authorities where the decision to approve bioequivalent products containing such pharmaceutical alternatives must be considered in the light of safety and efficacy, and more particularly, with respect to their substitutability. This article describes the various issues and contentions associated with the concept of pharmaceutical alternatives, specifically with respect to the uses of different salts and the implications for safety, efficacy and generic substitution.
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Spotlight on research: 50 years of Pharmaceutical Sciences Research Excellence Faculty of Pharmacy Rhodes University
- Authors: Walker, Roderick B
- Date: 2006
- Subjects: To be catalogued
- Language: English
- Type: text , article
- Identifier: http://hdl.handle.net/10962/184243 , vital:44193 , xlink:href="https://hdl.handle.net/10520/EJC81478"
- Description: This year, the Faculty of Pharmacy at Rhodes University is celebrating its 50th Anniversary. Over 2000 BPharm, 33 BSc honours, 65 MSc and 27 PhD degrees have been conferred since the Faculty’s inception. The diverse research activities and dedicated academic staff have ensured that the Faculty of Pharmacy has high visibility with respect to research outputs, as is evidenced by the appointment of various members of staff to national and international research, regulatory and professional committees, as well as to serving on the editorial boards of a number of international journals. In addition, staff regularly publish in international and local peer-reviewed journals and present their research findings at international and local conferences.
- Full Text:
- Authors: Walker, Roderick B
- Date: 2006
- Subjects: To be catalogued
- Language: English
- Type: text , article
- Identifier: http://hdl.handle.net/10962/184243 , vital:44193 , xlink:href="https://hdl.handle.net/10520/EJC81478"
- Description: This year, the Faculty of Pharmacy at Rhodes University is celebrating its 50th Anniversary. Over 2000 BPharm, 33 BSc honours, 65 MSc and 27 PhD degrees have been conferred since the Faculty’s inception. The diverse research activities and dedicated academic staff have ensured that the Faculty of Pharmacy has high visibility with respect to research outputs, as is evidenced by the appointment of various members of staff to national and international research, regulatory and professional committees, as well as to serving on the editorial boards of a number of international journals. In addition, staff regularly publish in international and local peer-reviewed journals and present their research findings at international and local conferences.
- Full Text:
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