Training

Mark Powell Scientific is accredited as a training provider by the UK’s National Skills Academy. We provide training in chromatography, spectroscopy, data integrity, pharmaceutical dissolution testing, technical report writing, basic laboratory skills and sample preparation. Mark was chosen to deliver a series of four 90 minute webinars on UV spectroscopy for Advanstar’s Spectroscopy Magazine during June 2014. He has also presented courses on pharmaceutical dissolution testing for Pharma Training, on liquid chromatography for Hichrom, and technical report writing for Inspired Pharma Training.

Our courses are designed to include a practical component and can be followed by formal assessment if required. Training can be tailored to each client’s needs depending on the equipment in use and the skills required by staff. Many clients find that it is more convenient to run training courses at their premises, since practical training can take place on the same equipment that analysts will be using routinely: travel and accommodation costs for trainees are also eliminated.

Courses at MP Scientific

The following descriptions give details of typical courses. Theory and practical content can be tailored according to need.

Sampling and Sample Preparation

The duration and content of this course will depend on the range of techniques covered. Topics include:

Overview of sample preparation techniques
Where to start – properties of analyte and matrix
Choice of sample container and sampling technique
Liquid-liquid extraction
Soxhlet extraction
Solid-phase extraction
Matrix solid-phase dispersion
Solid-phase micro-extraction (SPME)
Miniaturised techniques and QuEChERS approaches
Headspace sampling for gas chromatography
Sample derivatisation for chromatography
Practical exercises will be selected to provide experience of the techniques covered

Basic Laboratory Skills

In addition to running the on-site training course in basic laboratory skills, Mark Powell Scientific is willing to licence companies to use its training materials and train staff to deliver the course. The on-site course lasts two days and includes:

Measurement of mass
- Types of balance
- Calibration and daily checks
- Selecting and using the balance
- Choice of sample container
Measurement of volume
- Glass pipettes, automatic pipettes and volumetric syringes
- Volumetric flasks
- Burettes
- Calibration
pH measurement
- Definition of pH
- pH and temperature
- pH in non-aqueous or partly-aqueous solutions
- The pH electrode – use, care, calibration and maintenance
- pH indicator papers
Practical sessions:
- Practical sessions will be performed using a workbook to assess results against acceptance criteria. Exercises will include:
  - Setting up and calibrating a balance
  - Making up a standard solution
  - Preparing a series of calibration standards
  - Calibrating automatic and glass pipettes
  - Performing a titration
  - Preparing a buffer solution using a pH meter

Technical Report Writing

A two-day course on technical report writing including:

Organisation and structure
- Planning the report
- Accuracy, brevity and clarity
- Report structure
Style
- Rules of style and grammar
- Punctuation
- SI unit abbreviations
Graphical presentation of data
- Presenting data clearly in tables and figures
- Trend line and curve fitting
- Error bars
- Graphical representation of processes
Statistical methods
- Types of average
- Statistical distributions
- Deviations from normality
- Outliers
- Comparing means and variances
- Evaluating linearity
Practical sessions:
- Identifying errors in report extracts
- Designing tables and figures
- Writing a report using model data

Pharmaceutical Dissolution Testing

A three-day course on the theory and practice of dissolution testing including:

Purposes of dissolution testing
Dissolution theory, sink conditions and intrinsic dissolution rate
Dissolution and drug release testing apparatus
Requirements for different dosage forms (including data interpretation)
Dissolution equipment qualification
Dissolution method development including sampling time points and assay requirements
Dissolution method validation
- Setting method validation acceptance criteria with reference to drug product specifications
- Specificity, linearity/range, accuracy/recovery, precision, robustness and solution stability
Dissolution and the assessment of bioavailability/bioequivalence
Practical sessions: setting up a dissolution tester with basket and paddle apparatus; performing a dissolution test on an immediate release drug product

This course will benefit anyone requiring an intensive introduction to dissolution testing and the associated procedures working in the following areas:

Regulatory Affairs
Pharmaceutical Development
Analytical Development
Project Management
Quality Control
Quality Assurance

After completing this course, trainees will understand dissolution theory, be familiar with the different types of pharmaceutical dissolution testing equipment, be able to adopt a logical, scientifically-sound approach to method development, understand the application if in vitro dissolution data in assessing bioequivalence, and be able to perform a dissolution test using USP 1 or 2 dissolution apparatus.

Data Integrity

Data Integrity Awareness for Laboratory Analysts

A half-day course on data integrity for analytical chemists including:

Pharmaceutical quality: safety and efficacy
Background to data integrity: fraudulent data case studies
Consequences of fraud for companies and individuals
The requirements of data integrity
- Sampling and traceability
- Informal testing (e.g. trial injections)
- Computerised systems – including date stamps, audit trails and user accounts
- Laboratory data systems – data acquisition and processing methods
- Reporting and archiving results
Practical exercise – identifying potentially fraudulent data

Data Integrity Auditing

A one-day course on data integrity auditing including:

Introduction and fraudulent data case studies
Extracts of FDA warning letters relevant to data integrity
The requirements of data integrity
- Sampling and traceability
- Informal testing (e.g. trial injections)
- Computerised systems – including date stamps, audit trails and user accounts
- Laboratory data systems – data acquisition and processing methods
- Reporting and archiving results
Practical exercises
- Auditing laboratory records
- Auditing laboratory data systems
- Auditing LIMS systems

Chromatography

Introduction to HPLC/UHPLC

A one-day course on the fundamentals of liquid chromatography including:

Polarity, solubility, hydrogen bonding and pKa
Chromatographic theory
Retention mechanisms
Instrumentation:
- Degassers
- Pumps
- Column ovens
- Detectors
Mobile and stationary phases
Ion suppression and ion pairing
Practical exercises:
Mobile phase preparation
Column connection
System equilibration and wellness

HPLC/UHPLC Maintenance and Troubleshooting

A one-day course on maintaining and troubleshooting liquid chromatography systems including:

Revision of chromatographic theory
Peak characterisation: width, symmetry, height
System suitability parameters
Data from method development and validation studies as predictors of method performance
Problems caused by:
- Mobile phase
- Column
- Sample/standard preparation
- Pump
- Injector
- Detector & data system
Essential tools
Monitoring system performance
Preventative maintenance
Practical exercises:
- Revision of topics in the introductory course, plus:
- Sample filtration
- Priming a dry pump (e.g. after maintenance)
- Diagnosing leaks, blockages and pressure fluctuations

HPLC/UHPLC Method Development

A two-day course on method development for liquid chromatography including:

Revision of chromatographic theory
Nature of the analyte(s):
- Polarity/solubility
- Functionality
- Detectability
- Stability
Nature of the matrix:
- Analyte concentration
- Ease of extraction
- Chromatographic interference
Method requirements for accuracy, precision and sensitivity
Sample preparation approaches
Developing the separation
- Selection of initial conditions
- Sample concentration and injection volume
- Isocratic and gradient elution
- Optimising linearity, sensitivity, selectivity and resolution
- Strategies for ionic and non-ionic analytes
- Chiral separations
- Detector considerations
Biochemical separations
Method validation and transfer
Practical exercises:
- Trainees will develop two separations: the first will be for a binary mixture containing a polar molecule and a non-polar species; the second will be for a ternary mixture containing ionic and non-ionic analytes.

Introduction to Ion Chromatography

A one-day course on the fundamentals of ion chromatography including:

Chromatographic theory
Retention mechanisms in ion chromatography
Instrumentation:
- Degassers
- Pumps
- Column ovens
- Detectors (UV, electrochemical and conductivity)
Mobile and stationary phases
Suppression of background conductivity
Practical exercises:
- Mobile phase preparation
- Column connection
- System equilibration and wellness

Introduction to LC-MS

A one-day course on the fundamentals of LC-MS including:

Chromatographic theory
LC-MS system components
- Ion sources
- Vacuum system
- Ion optics
- Types and characteristics of mass analysers
- Ion detector types
Mobile phase considerations and limitations
Tuning and calibration
Maintenance
Qualitative and quantitative analysis
Practical exercises:
- Ion source cleaning
- Tuning and calibration
- Optimisation of ion source conditions

Spectroscopy

Ultraviolet Spectroscopy

A one-day course on the fundamentals of UV spectroscopy including:

The electromagnetic spectrum
Bonding orbital energy levels, pi bonds and conjugation
Electronic transitions and absorbance wavelengths
The Beer-Lambert Law
Spectrometer components and optical path designs
Sample cuvettes – selection, use and cleaning
Qualitative and quantitative analysis
Derivative spectroscopy
Typical applications
Practical exercise – instrument calibration and assay of an unknown sample

Fourier Transform Infrared Spectroscopy

A one-day course on the fundamentals of IR spectroscopy including:

The electromagnetic spectrum
Bond stretching, bending and rotation
Frequency, wavelength, wavenumber and band intensity
Absorbance regions associated with different functional groups
Spectrometer components and optical path designs
The interferogram
Sample preparation – thin film, KBr pellet and diamond ATR
Artefacts caused by carbon dioxide and water
Qualitative and quantitative analysis
Typical applications
Practical exercise – sample preparation and data acquisition

Interpretation of Infrared Spectra

A one-day course on the interpretation of IR spectra including:

Revision of modes of absorbance in the IR region
Appearance of typical functional group absorbance bands – spectral region and intensity
Positional isomers, including aromatic substitution patterns
Practical exercise – interpretation of unknown spectra

Mass Spectrometry

A one-day course on the fundamentals of mass spectrometry including:

The covalent bond
Bond strength and fragmentation
Deflection of ions in a magnetic field and mass:charge ratio
Components of a mass spectrometer – overview
Types of ion source, mass analyser and detector
Stable isotopes and monoisotopic masses of common elements
Mass resolution
Molecular formulae from accurate mass data
Large molecules and multiple charging
Interfaces for GC-MS and LC-MS
Practical exercise – sample preparation and data acquisition

Interpretation of Electron Ionisation Mass Spectra

A one-day course on the interpretation of mass spectra including:

Revision of basic theory and instrument design
Data produced by different ionisation methods and mass analysers
Typical EI mass spectra and common neutral losses
Identifying possible molecular ions
The odd nitrogen rule
Rings plus double bonds
Stable isotope patterns and molecular composition
Data from accurate mass determinations
Fragmentation and rearrangement mechanisms
Worked examples
Practical exercise – interpretation of unknown spectra