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RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 1
Use of DSC in Preformulations
A Seminar as a part of curricular requirement
for I year M. Pharm I semester
Presented by
G.kavya
(Reg. No. 20L81S0304)
Under the guidance/Mentorship of
Dr. Nawaz Mahammad., M.pharm,Ph.D.,
Associate Professor
Dept. of Pharmaceutics
RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 2
• Introduction of DSC
Principle of DSC
• Introduction of preformulations
• Uses of DSC in preformulation studies
• References
Contents
RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 3
 “DSC” stands for “ Differential scanning calorimetry” Most popular
thermal technique.
 DSC is a measures the heat absorbed or liberated during the various
transition in the sample due to temperature treatment.
 Different thermal events measured by DSC such as crystallization,
the onset of oxidation, melting, and heats of transition i.e. enthalpy
Introduction of DSC
RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 4
• DSC measurement are both qualitative and quantitative and provide
information about physical and chemical changes involving:
Endothermic process ,Exothermic process
• Measure difference in heat flow rate between a sample and inert
reference material as a function of time and temperature
Principle of DSC
RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 5
Pre-formulation studies can be define as an investigation of physical
and chemical property of a drug substance alone and when
combined with excipients
Pre-formulation can be considered as a critical decision making tool
during drug development and drug discovery
Objective:
To develop stable, effective and safe dosge forms.
To establish the physico – chemical parameters of a new drug
substance
To determine its kinetics and stability
Introduction of preformulations :
RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 6
• To determine the characterization of polymers
• To determine the difference between of crystalline and amorphous
form of a compound.
• To identify drug-excipient interactions
• To characterize crystalline nature of a compound
• To determine the dehydration/desolvation
• To determine heat of fusion
Use of DSC in preformulations
RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 7
Figure 1: A DSC plot for polyethylene terephthalate sample.
The plot illustrate both exothermic and endothermic thermal event that occurred a
temperature scan from 50°-300°c
To Determine the characterization of polymers:
RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 8
• To determine the different between crystalline and amorphous form of a
compound
Fig.2: DSC scan for a crystalline and amorphous pharmaceutical drug(Indomethacin) showing
the glass transition, crystallization, and melting peaks
RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 9
• To identify drug- excipient interactions
Fig 3:The DSC curves of drug with excipients, A)Dextrose
a)pure methyldopa b) pure excipient and c) binary mixture of methyldopa
RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 10
• A-a endothermic peak at 130.6°c corresponding to the lose of water from the crystalline
structure.
• The exothermic event followed by intense endothermic pack was observed at
approximately 315.45°c
• A-b indicated and endothermic melting peak at 167.50°c The mixture of methyldopa and
dextrose.
• A-c new peak at 89.91°c and the methyldopa melting event was disappeared completely.
• Since the peak of crystalline water loss can be observed at approximately 130°c -89.91°c
attributed to water elimination of methyldopa and dextrose reaction.
RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 11
• To characterize the crystalline nature of a compound
Fig 4: DSC curve of crystalline bisoprolol 1st heating, cooling (glass transition of
amorphised material) and 2nd heating (glass transition, cold crystallisation, melting
of re-crystallised material).all runs obtained at 10°c min heating rate.
RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 12
• To determine dehydration/desolvation
 Usually at lower temperatures
 Large enthalpy because of the
evaporation of released water/solvent
 may result in lower hydrates ,anhyd-
rates phases, and amorphous phase
RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 13
• To determine heat of fusion : DSC is commonly used to measure the
heat of fusion of a crystalline solid
Heat of fusion:
 Integrated area under melting curve
 may overlap with recrystallization
 may overlap with decomposition and
sublimation
RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 14
• Yoshihashi Y, Yonemochi E, Maeda Y, Terada K. predictionof the
induction period of crystallization of naproxen in solid dispersion
using differentitial scanning calorimetry. J Therm Anal calorim.
2010;99:15-9
• Hohne G,Hemminger W, Flammersheim H-J. Differential Scanning
Calimetry: Springer- Verlag, 1996
• Riga AT, Oberoi LM, Alexander KS. Differential scanning Calorimetry
as a preformulation tool for studying eutectics relevant in
pharmaceuticals. Am Phaem Rev. 2004;7:18-23
References
RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 15

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Use Of DSC in Preformulations

  • 1. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 1 Use of DSC in Preformulations A Seminar as a part of curricular requirement for I year M. Pharm I semester Presented by G.kavya (Reg. No. 20L81S0304) Under the guidance/Mentorship of Dr. Nawaz Mahammad., M.pharm,Ph.D., Associate Professor Dept. of Pharmaceutics
  • 2. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 2 • Introduction of DSC Principle of DSC • Introduction of preformulations • Uses of DSC in preformulation studies • References Contents
  • 3. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 3  “DSC” stands for “ Differential scanning calorimetry” Most popular thermal technique.  DSC is a measures the heat absorbed or liberated during the various transition in the sample due to temperature treatment.  Different thermal events measured by DSC such as crystallization, the onset of oxidation, melting, and heats of transition i.e. enthalpy Introduction of DSC
  • 4. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 4 • DSC measurement are both qualitative and quantitative and provide information about physical and chemical changes involving: Endothermic process ,Exothermic process • Measure difference in heat flow rate between a sample and inert reference material as a function of time and temperature Principle of DSC
  • 5. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 5 Pre-formulation studies can be define as an investigation of physical and chemical property of a drug substance alone and when combined with excipients Pre-formulation can be considered as a critical decision making tool during drug development and drug discovery Objective: To develop stable, effective and safe dosge forms. To establish the physico – chemical parameters of a new drug substance To determine its kinetics and stability Introduction of preformulations :
  • 6. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 6 • To determine the characterization of polymers • To determine the difference between of crystalline and amorphous form of a compound. • To identify drug-excipient interactions • To characterize crystalline nature of a compound • To determine the dehydration/desolvation • To determine heat of fusion Use of DSC in preformulations
  • 7. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 7 Figure 1: A DSC plot for polyethylene terephthalate sample. The plot illustrate both exothermic and endothermic thermal event that occurred a temperature scan from 50°-300°c To Determine the characterization of polymers:
  • 8. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 8 • To determine the different between crystalline and amorphous form of a compound Fig.2: DSC scan for a crystalline and amorphous pharmaceutical drug(Indomethacin) showing the glass transition, crystallization, and melting peaks
  • 9. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 9 • To identify drug- excipient interactions Fig 3:The DSC curves of drug with excipients, A)Dextrose a)pure methyldopa b) pure excipient and c) binary mixture of methyldopa
  • 10. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 10 • A-a endothermic peak at 130.6°c corresponding to the lose of water from the crystalline structure. • The exothermic event followed by intense endothermic pack was observed at approximately 315.45°c • A-b indicated and endothermic melting peak at 167.50°c The mixture of methyldopa and dextrose. • A-c new peak at 89.91°c and the methyldopa melting event was disappeared completely. • Since the peak of crystalline water loss can be observed at approximately 130°c -89.91°c attributed to water elimination of methyldopa and dextrose reaction.
  • 11. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 11 • To characterize the crystalline nature of a compound Fig 4: DSC curve of crystalline bisoprolol 1st heating, cooling (glass transition of amorphised material) and 2nd heating (glass transition, cold crystallisation, melting of re-crystallised material).all runs obtained at 10°c min heating rate.
  • 12. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 12 • To determine dehydration/desolvation  Usually at lower temperatures  Large enthalpy because of the evaporation of released water/solvent  may result in lower hydrates ,anhyd- rates phases, and amorphous phase
  • 13. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 13 • To determine heat of fusion : DSC is commonly used to measure the heat of fusion of a crystalline solid Heat of fusion:  Integrated area under melting curve  may overlap with recrystallization  may overlap with decomposition and sublimation
  • 14. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 14 • Yoshihashi Y, Yonemochi E, Maeda Y, Terada K. predictionof the induction period of crystallization of naproxen in solid dispersion using differentitial scanning calorimetry. J Therm Anal calorim. 2010;99:15-9 • Hohne G,Hemminger W, Flammersheim H-J. Differential Scanning Calimetry: Springer- Verlag, 1996 • Riga AT, Oberoi LM, Alexander KS. Differential scanning Calorimetry as a preformulation tool for studying eutectics relevant in pharmaceuticals. Am Phaem Rev. 2004;7:18-23 References
  • 15. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 15