Alclometasone dipropionate is a synthetic glucocorticoid corticosteroid and a corticosteroid ester. At is an Active raw material for different products in pharmaceutical industry.
CHEMICAL FORMULA
C23H37ClO7CHEMICAL STRUCTUREAlclometasone dipropionateDEFINITIONAlclometasone Dipropionate contains not less than 97.0% and not more than 102.0% of C23H37ClO7 calculated on the dried basis.
ASSAY (HPLC PROCEDURE)MOBILE PHASE:
Methanol and Solution A in ratio (2: 1)
SOLUTION A:
6.80 mg/ml of monobasic potassium phosphate (0.05 M)
INTERNAL STANDARD SOLUTION:
2 mg/ml of betamethasone dipropionate in methanol
STANDARD STOCK SOLUTION:
1.2 mg/ml of Alclometasone Dipropionate reference standard in methanol
STANDARD SOLUTION:
4.0 ml of Standard stock solution and 4.0 ml of Internal standard solution. Dilute with methanol to 25 ml. ( this solution contains 0.2 mg/ml of Alclometasone Dipropionate reference standard.)
SAMPLE STOCK SOLUTION:
1.2 mg/ml of Alclometasone Dipropionate in methanol
SAMPLE SOLUTION:
4 ml of Sample stock solution and 4 ml of Internal standard solution. Dilute with methanol to 25 ml.
CHROMATOGRAPHIC SYSTEMMode: LC
Detector: UV 254 nm
Column: 4-mm x 30-cm; packing L 1
Flow rate: 1.2 ml/min
Injection size: 10 µLRELATIVE STANDARD DEVIATION
Relative Standard Deviation should not be more than 2%.
CALCULATION
%age Assay = Hs/Ha × Ca/Cs × 100
Hs = Peak height ratio from the Sample solution
Ha = peak height ratio from the Standard solution
Ca = concentration of Alclometasone Dipropionate in the Standard solution (mg/ml)
Cs = concentration of the Sample solution (mg/ml)
ACCEPTANCE CRITERIA:
97.0% - 102.0% on the dried basis
IMPURITIES
INORGANIC
RESIDUE ON IGNITION:
Should be Not More Than 0.1%.
HEAVY METALS:
Should be Not More Than 30ppm.
Organic
HPLC-PROCEDUREMOBILE PHASE: Acetonitrile and water (3:2)
DILUENT: Acetonitrile and water (2:1)
SYSTEM SUITABILITY SOLUTION: 1.5 mg/ml of Alclometasone Dipropionate reference standard and 0.015 mg/ml of Alclometasone Dipropionate Related Compound in Diluent
SAMPLE SOLUTION: 1.5 mg/ml of Alclometasone Dipropionate in Diluent
CHROMATOGRAPHIC SYSTEMMode: LC
Detector : UV 254 nm
Column: 4.6-mm x 15-cm; 5 µm packing L1
Flow rate: 1 ml/min
Injection size: 5 µL
Run time: Three times the retention time of alclometasone
Tailing factor: NMT 1.5 for alclometasone dipropionate
Relative standard deviation: NMT 2.0% for alclometasone dipropionate
Resolution: NLT 2.0 between alclometasone dipropionate and alclometasone dipropionate related compound A
CALCULATION
Ai/Aa × 1/F × 100
Ai = Peak area for each impurity from the sample solution
Aa = Sum of all peaks from sample solution
F = Relative response factor
ACCEPTANCE CRITERIA:
Total impurities should be not more than 2.0%.
SPECIFIC TESTS
OPTICAL ROTATION :
Sample solution: 30 mg/ml in dioxane
Acceptance criteria: +21° to +25°
Loss on Drying: Dry a sample in a vacuum at a pressure not exceeding 5 mm of mercury at 105° for 3 h: