Development and validation of an ultrahigh-performance liquid chromatographic method for determination of nicotine in chewing gum
(2021) KASM01 20211Centre for Analysis and Synthesis
- Abstract
- Introduction: Validation of a new test method to determine nicotine from chewing gum extracts with ultra high-performance liquid chromatography.
Background: In Quality Control-laboratories, the methods that are regularly used are consistently developed in order to conduct effective analysis procedures. The aim of all of these developments is to simplify the analysis as much as possible and make the methods robust and efficient to maintain preciseness since they will be used continuously. Methods that do not fulfil all the requirements are usually replaced with new methods that are intended for this purpose. The two methods that are used to determine nicotine in chewing gum extracts do not fulfil the requirements for specificity and... (More) - Introduction: Validation of a new test method to determine nicotine from chewing gum extracts with ultra high-performance liquid chromatography.
Background: In Quality Control-laboratories, the methods that are regularly used are consistently developed in order to conduct effective analysis procedures. The aim of all of these developments is to simplify the analysis as much as possible and make the methods robust and efficient to maintain preciseness since they will be used continuously. Methods that do not fulfil all the requirements are usually replaced with new methods that are intended for this purpose. The two methods that are used to determine nicotine in chewing gum extracts do not fulfil the requirements for specificity and robustness, therefore a new method
that fulfil all the requirements was developed. The validation criteria and requirements were conducted from the validation SOP (Standard Operating Procedure) that is regulated with ICH (International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use) and USP (United States Pharmacopoeia) regulations.
Aim(s): The aim is to validate and develop the new method TMD-0000877 that is intended to be robust and selective for all the chewing gum formulations.
Methods: The instruments used in the older methods (named A and B) are based on HPLCanalysis where the latter method uses a column with a very low performance that results in peaks with low resolutions. Method B is only selective for two formulations, and the remaining formulations are analysed with method A. The new method uses an UHPLC (Ultra High-Performance Liquid Chromatography system) and is considered to be selective for all the 17 formulations. The validation experiment consists of testing different parameters such as robustness, specificity, precision, robustness, linearity, accuracy, method equivalency, and filter study. In order to assess the robustness, a 3-factorial DOE (Design of Experiment) was
done by randomly varying analysis parameters (flow, pH and temperature) giving a total of nine runs. All data were numerically calculated with Excel and Minitab.
Results: All the parameters fulfilled the requirements and most importantly the new method TMD-0000877 was selective for all the formulations since no interference under the nicotine peak was obtained. The robustness experiment gave contingent results since no significant difference was obtained for all the formulations. The only formulation that diverged was Spearmint 4 mg since a significant difference in analysis parameters was shown when the temperature is increased, due to a temperature sensitive colouring agent in the formulation that interfered with the nicotine peak, resulting in low resolution values. Although the robustness experiment fulfilled the requirements since all runs conducted a %RSD (Relative
Standard Deviation) ≤ 5.
Conclusion: The validation was successful, and all the tested parameters fulfilled the requirements. The method will be in use when the validation report is approved by McNeil AB and the countries demanding the method. (Less) - Popular Abstract
- A new method for determining nicotine in the chewing gum formulation used at the Quality-Control labs at McNeil AB, was developed and validated. The aim of this project was to replace several older methods with a robust and selective method for all the chewing gum formulations. The analysis instruments used for determining nicotine are liquid chromatography, which is a process for separating components by pumping a solvent mixture at high pressure through a solid silica particle-packed column in order to separate and determine compounds. The chewing gum formulation consists of a total of 17 flavours and strengths, and the sample preparation method included dissolving and chewing the gums in media in a chewing apparatus.
The aim of this... (More) - A new method for determining nicotine in the chewing gum formulation used at the Quality-Control labs at McNeil AB, was developed and validated. The aim of this project was to replace several older methods with a robust and selective method for all the chewing gum formulations. The analysis instruments used for determining nicotine are liquid chromatography, which is a process for separating components by pumping a solvent mixture at high pressure through a solid silica particle-packed column in order to separate and determine compounds. The chewing gum formulation consists of a total of 17 flavours and strengths, and the sample preparation method included dissolving and chewing the gums in media in a chewing apparatus.
The aim of this project was to develop and validate the new test method using validation approaches dedicated for the pharmaceutical industry. The validation consisted of testing different parameters that explained the robustness of the method, specificity, precision, linearity, method equivalency, filter study, accuracy, and solution stability. The requirements for each parameter were taken from the validation SOP (Standard Operating Procedure) that belongs to the company.
The results obtained from the experiments showed that the method fulfilled all the requirements, was selective for all the formulations and was robust. Since all the other validation parameters also fulfilled the criteria, the method will be applicable when the validation report is written and approved. (Less)
Please use this url to cite or link to this publication:
http://lup.lub.lu.se/student-papers/record/9057720
- author
- Hojeij, Zeinab LU
- supervisor
- organization
- course
- KASM01 20211
- year
- 2021
- type
- H2 - Master's Degree (Two Years)
- subject
- keywords
- Chewing gum, Nicorette®, Nicotine, Ultra High-Performance Liquid Chromatography, Validation, Technical analytical chemistry
- language
- English
- id
- 9057720
- date added to LUP
- 2021-06-28 16:03:44
- date last changed
- 2021-06-28 16:03:44
@misc{9057720,
abstract = {{Introduction: Validation of a new test method to determine nicotine from chewing gum extracts with ultra high-performance liquid chromatography.
Background: In Quality Control-laboratories, the methods that are regularly used are consistently developed in order to conduct effective analysis procedures. The aim of all of these developments is to simplify the analysis as much as possible and make the methods robust and efficient to maintain preciseness since they will be used continuously. Methods that do not fulfil all the requirements are usually replaced with new methods that are intended for this purpose. The two methods that are used to determine nicotine in chewing gum extracts do not fulfil the requirements for specificity and robustness, therefore a new method
that fulfil all the requirements was developed. The validation criteria and requirements were conducted from the validation SOP (Standard Operating Procedure) that is regulated with ICH (International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use) and USP (United States Pharmacopoeia) regulations.
Aim(s): The aim is to validate and develop the new method TMD-0000877 that is intended to be robust and selective for all the chewing gum formulations.
Methods: The instruments used in the older methods (named A and B) are based on HPLCanalysis where the latter method uses a column with a very low performance that results in peaks with low resolutions. Method B is only selective for two formulations, and the remaining formulations are analysed with method A. The new method uses an UHPLC (Ultra High-Performance Liquid Chromatography system) and is considered to be selective for all the 17 formulations. The validation experiment consists of testing different parameters such as robustness, specificity, precision, robustness, linearity, accuracy, method equivalency, and filter study. In order to assess the robustness, a 3-factorial DOE (Design of Experiment) was
done by randomly varying analysis parameters (flow, pH and temperature) giving a total of nine runs. All data were numerically calculated with Excel and Minitab.
Results: All the parameters fulfilled the requirements and most importantly the new method TMD-0000877 was selective for all the formulations since no interference under the nicotine peak was obtained. The robustness experiment gave contingent results since no significant difference was obtained for all the formulations. The only formulation that diverged was Spearmint 4 mg since a significant difference in analysis parameters was shown when the temperature is increased, due to a temperature sensitive colouring agent in the formulation that interfered with the nicotine peak, resulting in low resolution values. Although the robustness experiment fulfilled the requirements since all runs conducted a %RSD (Relative
Standard Deviation) ≤ 5.
Conclusion: The validation was successful, and all the tested parameters fulfilled the requirements. The method will be in use when the validation report is approved by McNeil AB and the countries demanding the method.}},
author = {{Hojeij, Zeinab}},
language = {{eng}},
note = {{Student Paper}},
title = {{Development and validation of an ultrahigh-performance liquid chromatographic method for determination of nicotine in chewing gum}},
year = {{2021}},
}