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Analytical Chemistry and Validation Training Courses – 2010

Presented at Your Facility

Presented By Gregory McLaughlinCEO/Chief Analytical Development Scientist

West Palm Beach Analytical Development, LLC (WPBAD)

561-601-9730 (Phone) [email protected] (email) or

[email protected] (email) http://www.wpbad.biz/ (website)

WPBAD Course Agendas

mailto:[email protected]�

mailto:[email protected]�

http://www.wpbad.biz/�

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Course Offerings


Subject Title Page #CE HPCE basics, method development concepts, use of CE/HPLC, and studies 3

DSC/DTA Differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA) 4

DissolutionIntroduction to dissolution testing - overview, design, calibration,

troubleshooting, and automation of dissolution test equipment 5

Extractables/Leachables

Development of extractables/leachables methods using a systematic approach 6

FTIRIntroduction into IR and FTIR - infrared (IR) and fourier transform infrared (FTIR) spectroscopy 7

GCIntroduction into GC - gas chromatography (GC) – an overview of one

of the most heavily used analytical chemistry techniques 8

HPLCIntroduction to HPLC – an overview of the most versatile

analytical chemistry technique in the world 9

HPLCAdvanced reverse phase HPLC method development concepts –

development of a robust HPLC method 10

HPLCHPLC troubleshooting and preventive maintenance – diagnosing and

fixing problems with your HPLC system and method 11

HPLC HPLC valve switching - imagineering with switching valves 12Method ValidationCurrent method validation and instrument qualification issues 13

pH Introduction to pH 14Stress Studies Stress studies- including use and optimization of the PDA detector 15

UV/Vis Spectroscopy

UV/Visible spectroscopy 16

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CE Schematic CE Theory CE injection techniques Capillary length and diameter effects Voltage effects Temperature effects pH effects Ionic strength effects Organic modifier effects Micellar Electrokinetic Capillary Chromatography (MECC) Uses of CE and HPLC as Orthogonal Techniques Buffer additive effects Ion pairing agent effects HISFACE concentration technique for increasing sensitivity Use of CE for monitoring studies Conclusions

HPCE Basics, Method Development Concepts, Use of CE/HPLC, and Studies (Agenda)


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Differential Scanning Calorimetry (DSC)and Thermal Gravimetric Analysis (TGA) Agenda

References Concept of thermal analysis Differential Thermal Analysis (DTA) Differential Scanning Calorimetry (DSC) Crystallization and melting Glass transition Thermogravimetric (TGA) Analysis Questions


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Introduction to Dissolution Testing- Overview, Design, Calibration, Troubleshooting, and Automation of Dissolution Test Equipment (Agenda)

Dissolution testing overview Dosage forms to be tested Official dissolution monographs Official dissolution apparatus Which type of dissolution apparatus for which type of sample? Apparatus 1 – 7 Qualification of dissolution systems Mechanical calibration parameters Apparatus suitability test (USP) Troubleshooting Automation Questions


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Development of Extractables/Leachables Methods Using

a Systematic Approach (Agenda) The importance of extractables and leachables testing for a

successful product launch Top ten reasons why controlled extraction studies are needed What does drug packaging do? Definitions - extractables and leachables Industry guidance Extractables method development including examples Extractables method validation Leachables method development including examples Leachables method validation Approaches for inhalation solution products Case studies


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Introduction into IR and FTIR - Infrared (IR) and Fourier Transform Infrared (FTIR) Spectroscopy (Agenda)

Acknowledgement Electromagnetic spectrum Principles of FTIR Different types of vibration IR Equation and characteristic frequencies IR versus UV IR instrument Interferometer and fourier transformation IR sample preparation Interpreting IR spectra Applications Questions


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Introduction into GC - Gas Chromatography (GC) –An Overview of One of the Most Heavily Used

Analytical Chemistry Techniques (Agenda)

Chromatography and GC GC equipment (gas controller, syringe, autosamplers, inlet, oven,

column, detector (s), data analysis system) Injection techniques (split/splitless, headspace, purge and trap) Inlets, ovens, columns Chromatographic terminology ( efficiency, resolution, tailing

factor , asymmetry, and capacity factor) GC stationary phases Column specificity, length, diameter, phase ratio Flow rate, temperature effects Detectors (FID, TCD, EDC, Other) GC method development Applications Questions


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Chromatography and HPLC HPLC equipment (solvent reservoir, pump, injection

valve, column, detector (UV detector, DAD, refractive index, fluorescence, conductivity, electrochemical detector, evaporative light scattering detector, chiral detector, radioactive detector, mass spectrometry detector [MSD])

Chromatographic terminology ( efficiency, resolution, tailing factor , asymmetry, and capacity factor)

Maintaining a chromatographic separation Modes of chromatography (adsorption, sizing , ion

exchange, ion chromatography, hydrophobic interaction, and reverse phase)

Conclusions

Introduction to HPLC – An Overview of the Most Versatile Analytical ChemistryTechnique in the World (Agenda)


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Reverse Phase HPLC Method Development Concepts- Development of a Robust HPLC Method (Agenda)

Reverse phase chromatography Solubility and solvent mixtures Hydrophobic/hydrophilic interactions Effect of organic modifier concentration Flow rate and column length Fast separations pKa and ionization control of pH Ion pairing Ionic strength Temperature Use of diode array detector for detection and purity evaluation Other examples, spiking, method of standard addition, etc. Deformulation-multiple strategies applied to a complex pain reliever Use of CE/HPLC as orthogonal techniques Conclusions


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HPLC Troubleshooting and PreventiveMaintenance – Diagnosing and Fixing Problems with

Your HPLC System and Method (Agenda)

Theoretical plates, resolution, tailing factor, peak asymmetry factor Peak broadening (chromatographic, volume, solvent effects) Problems with the HPLC liquid flow path (dead volume, column

plugging, HPLC plumbing, column voids) Drip, drip, drip - are leaks inevitable? Retention Time Reproducibility Problems Other HPLC phenomena Systematic troubleshooting Avoiding potential disastrous results Software Situations Keeping your HPLC happy! Questions


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What are automated fluidics instruments for chromatography 6-Position/7-Port and 2-Position/6-Port low pressure selector valves 2-Position/6-Port high pressure valves 3-Position/7-Port with purge valves 2-Position/10-Port selector valves 10-Position/11-Port selector valves 8-Position/17-Port Stream selector valves Dissolution sampling 6 Column selector valves Conclusions

HPLC Valve Switching - Imagineering with Switching Valves (Agenda)


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Acknowledgments FDA 483s - quality and laboratory issues Current method validation and instrument

qualification practices Qualification of HPLC systems (DQ/IQ/OQ/PQ) FDA’s expectations FDA 483s - quality and laboratory issues Laboratory method flow Method validation (precision, accuracy, limit of

detection, limit of quantitation, specificity, linearity and range, ruggedness, robustness, and system suitability)

Conclusions

Current Method Validation and Instrument Qualification Issues (Agenda)


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Invention of pH pH - definition The pH scale Introduction to pH pH measurement Temperature compensation pH Meter – components, use, and calibration How Does a pH meter measure H+ concentration? Calibrating a pH Meter and buffers Reading samples Maintenance of pH meter Litmus paper

Introduction to pH (Agenda)


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Stress Studies- Including Use and Optimizationof the PDA Detector (Agenda)

Stress study overview Why do we perform stress studies? How to perform forced degradation studies in the lab Specificity and selectivity Stability-indicating assay development Regulatory guidance SOPs regarding stress studies Do’s and don’ts of stress studies Stress mechanisms: heat, oxidation, base, acid, and

light Use of diode array detector for detection and purity

evaluation Peak purity Stress pathways Conclusion


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UV/Visible Spectroscopy (Agenda) Spectroscopy and spectrophotometry Ultraviolet and visible spectroscopy Electronic transitions Spectra Transmission and color UV/Vis spectrophotometer and diode spectrophotometer schematics Detectors and cells Sources of noise Lamp and calibration solution spectra The spectral process and uses Overcoming/recognizing instrumental and spectral limitations Questions


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