Trigonometry Lab Report

S. DRUG SUBSTANCE
S1. General Information
S1.1 Nomenclature
Table 84 Nomenclature of Drug Substance
International Nonproprietary Name (INN) Levofloxacin Hemihydrate
Chemical Name 7H-Pyrido[1,2,3-de]-1,4-benzoxazine-6-carboxylic acid, 9-fluoro-2,3-dihydro-3-methyl-10-(4-methyl-1-piperazinyl)-7-oxo-hydrate (2:1), (S)-.(-)-(S)-9-Fluoro-2,3-dihydro-methyl-10-(4-methyl-1-piperazinyl)-7-oxo-7Hpyrido[1,2,3-de]-1,4-benzoxazine-6-carboxylic acid, hemihydrates
Generic name Levofloxacin Hemihydrate
CAS Number [138199-71-0]

S1.2 Structure and attachment for structure of drug substance
Table 85 Structure of Drug Substance
Structural Formula : C18H20FN3O4 •½ H2O
Relative Molecular Mass : 370.38
Structural Formula

:

S1.3

The reaction mixture is condensed under reduced pressure concentration. Then the reaction mixture is filtered in the presence of chloroform and charcoal.
• Neutralization and extraction step is done by mixing reaction mixture with Hydrochloric acid, Sodium hydroxide in drinking water and chloroform followed by dissolution and crystallization to form Crude Levofloxacin.
• Crude Levofloxacin is decolorized by ethanol and charcoal which is then recrystallized and centrifuged to form Levofloxacin (Intermediate).

Stage III: Preparation of Levofloxacin
Levofloxacin (Intermediate) undergoes dissolution and decoloration in presence of ethanol and charcoal followed by recrystallization and centrifugation to form Levofloxacin.
Stage IV: Drying and Packaging
The final product is dried, crushed and analyzed followed by inner packaging and outer packaging.

Fig. 18 The chemical synthetic route from Levofloxacin and ethyl ester (i.e. starting material to Levofloxacin

NO 2565 MFG. DATE: MM/YYYY
MANUFACTURED BY: XYZ PHARMACEUTICALS LTD
Sr. No. Test Observation Limit C015-1004001 C015-1004002 C015-1004003
01
Description Conform Conform Conform Light yellowish-white to yellow-white crystal or crystalline powder
02 Identification
(A) IR
(B) HPLC
Conform
Conform
Conform
Conform
Conform
Conform (A) Conform to standard spectrum
(B) Conform to Standard peak
03 Specific rotation -100° -101° -101° -92° to 106°
04 Water 2.4% 2.5% 2.4% 2.1% to 2.7%
05 Residue on ignition 0.02% 0.02% 0.02% NMT 0.2%
06 Heavy metals Conform Conform Conform NMT 10ppm
07 Impurities Impurity a 0.03% 0.03% 0.04% NMT 0.3% Impurity b 0.01% 0.02% 0.03% NMT 0.3% Impurity c 0.04% 0.04% 0.04% NMT 0.3% Impurity d ND ND ND NMT 0.3% Impurity e 0.06% 0.06% 0.06% NMT 0.8% Unknown impurity 0.02% 0.02% 0.02% NMT 0.1%

Total impurity (except impurity e) 0.11% 0.12% 0.14% NMT 0.5%
08 Residual Solvent
Methanol
Ethanol
Chloroform

0.0008%
0.04%
ND

0.0006%
0.03%
ND

0.0005%
0.02%
0.14%

NMT 0.1%
NMT 0.3%
NMT 0.006%
09 Assay 100.8% 100.3% 100.5% 98.5% to 102.0%

S4.5. Justification of