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UV-VIS
Spectroscopy for
Dissolution
Testing
Thomas Klink
October 29, 2008
8450
Introduced 1979
8451
Introduced 1984
8452A
Introduced 1986
8453
Introduced 1995
Detector
Sample
Exit slit
Dispersion
element
Dispersion element
Entrance slit
Reversed Optics
Room light cannot reach detectors
– narrow “acceptance angle” after sample
– geometry of spectrograph
Easy and convenient access
– better productivity
– Less error prone
Easy installation of accessories
– room light is not a problem
– Simple installation of accessories
Security Security
Pack Pack
Dissolution Biochemical
Testing Advanced Analysis
Dissolution Testing Advanced Kinetics
Multibath Dissolution (Deletes Execute
Thermal Denaturation
Advanced Method)
Testing
Combined Reports
General Purpose
Verification &
Standard Execute Advanced
Diagnostics
Dissolution bath
Vessel washing and filling
Partners Tablet dropping
Sampling system
Transfer from vessel to measurement system
Measurement system
Agilent Analytical measurement on sample
Data evaluation / report generation
Conversion of measured parameters
Output of dissolution results
Sample
transfer
8453
Spectrophotometer
RS232
HPIB
Data
ChemStation transfer Bath “Driver”
DDE Connection DDE Connection
Samples Standards
Measure
Measure
Standards
Samples
Process
Process Samples
Standards
Analytical Calibration
Results Result
Dissolution
Results Method
Standard
• Unlimited number of standards
• Choice of four calibration curve types
• Single, average or three-point background correction
Advanced
• Any combinations of wavelengths
• Any spectral processing (e.g. derivative + smooth)
• Least squares or Maximum Likelihood fit
• Single or multi-wavelength values
Off-line
– Manual
– Sipper
– Autosampler
On-line
– Multicell based sampling UV-visibleChemStation
– Valve based sampling dissolution run time
control
– Multibath with up to four baths
- Each bath is independent and may run a different method
Fully automated
– In combination with Caliper MultiDose
Multichannel
Pump
GP-IO
Blank Control
MCT
8453
Spectrophotometer
GP-IB or PC 1 2 3 4 5 6
Printer LAN Dissolution Vessels
Parallel
Advantages
– Fast cycle time (< 2 min)
– No lost medium
– Simultaneous sampling
(compatible with "basket" method)
Disadvantages
– Multiple flow cells
– Most expensive sampling system
• 8-port valve
– now improved for better reliability
• Powerful, variable flow rate pump
– adjustable to desired flow rate
GP-IO Valve
Valve/Pump 8 1 2
Controller 7 3
6 5 4
8453
Spectrophotometer
GP-IB PC
Printer
1 2 3 4 5 6
Dissolution Vessels
Serial/Parallel
Advantages
– Single cell
– Reliable
– Lowest cost
Disadvantages
– Relatively slow (5, 7.5 or 10 min cycle)
– Lost medium
– Potential sample carryover
– Vessel-to-vessel delay
(may be incompatible with "basket" method)
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