Alclometasone Dipropionate

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 C₂₃H₃₇ClO₇ CHEMICAL STRUCTURE

DEFINITION Alclometasone 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 SYSTEM Mode: LC Detector: UV 254 nm Column: 4-mm x 30-cm; packing L 1 Flow rate: 1.2 ml/min Injection size: 10 µL  RELATIVE 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-PROCEDURE MOBILE 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 SYSTEM Mode: 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:

It loses NMT 0.5% of 1ts weight.