A.

REFERENCE
National Formulary 32, 2014 p.6038

B. PROCEDURE
1. DESCRIPTION
a. Material
-
b. Procedure
Determine form, color, odor and taste of sample by visual or organoleptic examination.

2. SOLUBILITY
a. Material
Water
Alcohol

b. Procedure
For material and procedure see General Test Procedure Solubility, ANA-GT-027-xx.

3. CLARITY AND COLOR OF SOLUTION

a. Material
Water
b. Procedure
A solution of 1 g in 10 mL of boiling water is clear and nearly colorless.
Determine the absorbance of this solution at a wavelength of 400 nm.
Observe using spectrophotometer spectrum

4. IDENTIFICATION
Test A
a. Material
-
b. Procedure
Put the sample in the FT IR sample compartment.
Lower the pressure module until the desired pressure is achieved.
Record the spectra of the sample and standard over the range from about 4000 cm -1 and 450 cm-1
using Spectrum v2.00 software.
Do the same step for Lactose in-house standard.
Comparethe IR Spectrum of the sample and standard.

Test B
a. Material
DiluentPrepare a mixture of methanol and water (3:2).
Developing solvent Prepare a solution consisting of a mixture of ethylene dichloride, glacial
acetic acid, methanol, and water (50:25:15:10).
Standard solution A Prepare a solution of USP Lactose Monohydrate RS in Diluent having a
known concentration of 0.5 mg per mL.
 Standard solution B Prepare a solution of USP Dextrose RS, USP Lactose Monohydrate RS,
USP Fructose RS, and USP Sucrose RS in Diluent having a known concentration of 0.5 mg per
mL for each Reference Standard.
Test solution Transfer about 25 mg of Lactose Monohydrate to a 50-mL volumetric flask,
dissolve in and dilute with Diluent to volume, and mix.

b. Procedure
Thin-layer chromatographic plate (see Chromatography 621 ) coated with a 0.25-mm layer of
chromatographic silica gel. Allow the spots to dry, and develop the plate in a paper-lined
chromatographic chamber equilibrated with Developing solvent for about 1 hour prior to use.
Allow the chromatogram to develop until the solvent front has moved about three-quarters of the
length of the plate. Remove the plate from the chamber, dry in a current of warm air, and
redevelop the plate in fresh Developing solvent.
Remove the plate from the chamber, mark the solvent front, and dry the plate in a current of
warm air. Spray the plate evenly with a solution containing 0.5 g of thymol in a mixture of 95 mL
of alcohol and 5 mL of sulfuric acid.
Heat the plate at 130 for 10 minutes: the principal spot obtained from the Test solution
corresponds in appearance and RF value to that obtained from Standard solution A.
The test is not valid unless the chromatogram obtained with Standard solution B shows four
clearly discernible spots, disregarding any spots at the origin.
Test C
a. Material
Water
Ammonium hydroxide
b. Procedure
Dissolve 250 mg in 5 mL of water. Add 3 mL of ammonium hydroxide, and heat in a water bath

at 80 C for 10 minutes.
Observe test result

5. SPECIFIC ROTATION
a. Material
Water
6 N ammonium hydroxide.
b. Procedure

Dissolve 10 g by heating in 80 mL of water to 50 C, Allow to cool, and add 0.2 mL of 6 N ammonium

hydroxide.
Allow to stand for 30 minutes, and dilute with water to 100 mL.
Read the rotation of this solutio as a blank in 2-cm cells using polarimeter

Computation
Specific rotation =

spl - bl 1
x DF x = . o
Wspl d
 Where :
spl = Rotation of sample
bl = Rotation of the blank
Wspl = Weight of sample (g)
DF = Dilution factor of sample (100)
d = Diameter of the cell (2)

6. MICROBIAL LIMIT
See Prosedur Tetap Uji Mikrobiologi (QC3-SOP-04/xx).
See Prosedur Tetap Pengujian Total Plate Count dan Kuman Pathogen (QC3-SOP-44/xx).

7. ACIDITY OR ALKALINITY
a. Material
Water
6 N ammonium hydroxide.
b. Procedure
Dissolve 6 g by heating in 25 mL of carbon dioxide-free water, cool, and add 0.3 mL of
phenolphthalein TS.
Observe the test result.
 8. LOSS ON DRYING
For material and procedure see Test Procedure Loss on Drying, ANA-GT-010-x.
Condition test : Dry it at 80oC for 2 hours.

9. WATER, METHOD I
For material and procedure see General Test Procedure of Water Determination(Karl Fischer Method),
ANA-GT-018-x.

10. RESIDUE IN IGNITION

For material and procedure see Test Procedure Residue on Ignition, ANA-GT-012-x.

Condition: a specimen ignited at a temperature of 600 25 C.

11. HEAVY METALS (METHOD I)

For material and procedure see General Test Procedure of Heavy Metals Limit Test, ANA-GT-004-x.
Condition : Dissolve 4 g in 20 mL of warm water, add 1 mL of 0.1 N hydrochloric acid, and dilute with
water to 25 mL.

12. PROTEIN AND LIGHT- ABSORBING IMPURITIES

Measure the light absorption of a 1% (w/v) solution in the range of 210 to 300 nm.
Observe using spectrophotometer spectrum.

Prepared by: Checked/Approved by:

Lina Herlina Ponelta Bangun

QC Unit Head QC Responsible Pharmacist