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 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 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 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 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

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 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
spectrioscopy 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