Common Pharmacopeial Calculations

in USP Monographs
(Pharmacopeial Forum vol.31(2) [Mar.-Apr. 2005])

Miscellaneous tests : loss on drying , loss on ignition

Assays
Related compounds (chromatographic purity)

Miscellaneous tests : loss on drying , loss on ignition

Loss on drying

% LOD

%LOD = [(T-F)/(T-C)] x 100

Loss on ignition

% LOI

%LOI = [(T-F)/(T-C)] x 100

Assay
Assay as is
Calculation = Q/T x 100 = 495 / 500 x 100 = 99.0%
Assay dried basis

LOD

anhydrous basis
water
Assay result = [Q/T/(100-A/100)] x 100
= [295.0/300.0/(100-0.34)/100] x 100 = 98.7%
Assay on ignition basis
Assay result = [Q/T/(100-A/100)] x 100
= [96.0/99.8/(100-3.54)/100] x 100 = 99.7%

Assay result on previously dried basis

Calculation = Q/T x 100 = 10.7 / 10.5 x 100 = 101.9%

Assay result calculated on the anhydrous and solvent-free basis

Calculation = [Q/T/(100-A-B)/100] x 100
= 26.0 / 25.9/(100-0.183-0.281)/100]x100
= 101.9%

Common Calculation for Determination of the Assay Result

Chromatography : HPLC, GC
50C(ru/rs), DC(ru/rs), (301.39/337.84)(50C)(ru/rs)

Spectroscopy and other methods

IR , UV , polarography
10C(Au/As), P (Ws/Wu) (iu/is)

Determination of equivalence factor in titration-based assay

A + B
Acid-base titration
Redox titration
Titration
Direct titration
Residue or Back titration

products

Electron transfer

Titration
Direct titration
Assay result = [(V-B) x N x F x 100]/[TN x W x(100-A)/100] x100
= [(8.5-1.4)x0.11x25.43x100]/[0.1x202x(100-0.42)/100]
= 98.7%
Residue or Back titration
Assay result = [(B-V) x N x F x 100]/[TN x W] x100 =
= [(43.78-15.10)x0.9993x30.05x100]/[1.0x1007.8]
= 99.7%

Related compounds or chromatographic impurity

Impurity in New Drug Substance
- Inorganic impurities
- Residue solvent
- Organic impurities
HPLC , GC
)Total peak area : 100(ri/rs)
)Different concentration of the test sample: 100ri/(rs+5ru)
)Using reference standard : 0.1(Cs/Cu)(ru/rs)
)Using relative response factors (RRF) : 100F(Cs/Cu)(ru/rs)

Recommendations
1. Present all terms
2. Its origin should be clearly explained
3. Dilution factor
4. Including the RRF and RRT in the monograph
5. Change 1 -4 as early as possible
6. Formulas are expressed in the same unit as in the
assay
7. Create the new chapter for clarification of the
calculation

THANK for your attention

DISCUSSION
SUGGESTION
QUESTION ? ? ? ?