Amoxicillin Hydrate

Amoxicillin

is a semisynthetic aminopenicillin antibiotic with bactericidal activity. It is used as Amixicillin Hydrate Amoxicillin binds to and inactivates penicillin-binding protein (PBP) 1A located on the inner membrane of the bacterial cell wall.

IUPAC  Name

IUPAC name of Amoxicillin Hydrate is (2S,5R,6R)-6-[[(2R)-2-amino-2-(4-hydroxyphenyl)acetyl]amino]-3,3-dimethyl-7-oxo-4-thia-1-azabicyclo[3.2.0]heptane-2-carboxylic acid, trihydrate 

Molecular Formula

C16H19N3O5S • 3H2O

Chemical Structure

Amoxicillin
Amoxicillin Hydrate

Formula Weight

419.4 

Purity

≥98%

Physical Appearance:

Amoxicillin Hydrate occurs as white to light yellowish white, crystals or crystalline powder.

Solubility

It is slightly soluble in water and in methanol, and very slightly soluble in ethanol (96%).

Identification

Determine the infrared absorption spectrum of Amoxicillin Hydrate as directed in the potassium bromide disk method under Infrared Spectrophotometry , and compare the spectrum with the Reference Spectrum or the spectrum of Amoxicillin RS: both spectra exhibit similar intensities of absorption at the same wave numbers.

Optical rotation

+290°   to   +315° (0.1 g calculated on the anhydrous basis, water, 100 mL, 100 mm).

Heavy metals

To 1.0 g of Amoxicillin Hydrate add 2 mL of a solution of magnesium sulfate heptahydrate (1 in 4), mix, and heat on a water bath to dryness. Carbonize the residue by gently heating. After cooling, add 1 mL of sulfuric acid, heat carefully, then heat at 500°C – 600°C to incinerate. After cooling, add 1 mL of hydrochloric acid to the residue, and heat on a water bath to dryness. Then add 10 mL of water to the residue, and heat on a water bath to dissolve. After cooling, add ammonia TS to adjust the pH to 3 – 4, and add 2 mL of dilute acetic acid. If necessary, filter, wash the residue on the filter with 10 mL of water, transfer the filtrate and washings into a Nessler tube, add water to make 50 mL, and use this solution as the test solution. Prepare the control solution as follows: To 2.0 mL of Standard Lead Solution add 2 mL of a solution of magnesium sulfate heptahydrate (1 in 4), then proceed in the same manner as for preparation of the test solution (not more than 20 ppm).

Water:

Not less than 11.0% and not more than 15.0% (0.1 g, volumetric titration, direct titration).

Assay

Weigh accurately an amount of Amoxicillin Hydrate and Amoxicillin RS, equivalent to about 30 mg (potency), dissolve each in a solution of boric acid (1 in 200) to make exactly 100 mL, and use these solutions as the sample solution and standard solution. Perform the test with exactly 10 mL each of the sample solution and standard solution as directed under Liquid Chromatography according to the following conditions, and calculate the peak areas, AT and AS, of amoxicillin in each solution. Amount [µg (potency)] of amoxicillin (C16H19N3O5S)   = MS × AT/AS × 1000 MS = Amount [mg (potency)] of Amoxicillin RS taken

Operating conditions:

Detector:

An ultraviolet absorption photometer (wavelength: 230 nm).

Column:

A stainless steel column 4.6 mm in inside diameter and 15 cm in length, packed with octadecylsilanized silica gel for liquid chromatography (5 µm in particle diameter).

Column temperature:

A constant temperature of about 25°C.

Mobile phase:

Dissolve 1.361 g of sodium acetate trihydrate in 750 mL of water, adjust to pH 4.5 with   acetic acid, and add water to make 1000 mL. To 950 mL of this solution add 50 mL of methanol.

Flow rate:

Adjust so that the retention time of amoxicillin is about 8 minutes.

System performance:

When the procedure is run with 10 µL of the standard solution under the above operating conditions, the number of theoretical plates of the peak of amoxicillin is not less than 2500.

System repeatability:

When the test is repeated 6 times with 10 µL of the standard solution under the above operating conditions, the relative standard deviation of the peak area of amoxicillin is not more than 1.0%.

Containers and storage Containers:

Tight containers at Room temperature

Stability

≥ 2 years

Note before using Amoxicillin Product:

Do not use this medication if you are allergic to amoxicillin or to any other penicillin antibiotic, such as ampicillin, dicloxacillin, oxacillin, penicillin, and others. Before using amoxicillin, tell your doctor if you are allergic to cephalosporins such as Omnicef, Cefzil, Ceftin, Keflex, and others. Also tell your doctor if you have asthma, liver or kidney disease, a bleeding or blood clotting disorder, mononucleosis (also called "mono"), or any type of allergy. Amoxicillin can make birth control pills less effective. Ask your doctor about using a non-hormone method of birth control (such as a condom, diaphragm, spermicide) to prevent pregnancy while taking this medicine. Take this medication for the full prescribed length of time. Your symptoms may improve before the infection is completely cleared. Amoxicillin will not treat a viral infection such as the common cold or flu. Do not share this medication with another person, even if they have the same symptoms you have. Antibiotic medicines can cause diarrhea. This may happen while you are taking amoxicillin, or within a few months after you stop taking it. This may be a sign of a new  infection. If you have diarrhea that is watery or bloody, stop taking this medicine and call your doctor. Do not use anti-diarrhea medicine unless your doctor tells you to. Related Posts:
  1.    EDTA          2.  Diclofenac Sodium            3.   Vitamin "C"

Testing of Vitamin “C” in a drug

Here is the titration method for testing of Vitamin "C "in a supplement drug. It becomes more difficult to test Vitamin "C" in drug having Other vitamins like Vitamin "A ", Vitamin "E " Vitamin B", extracts like Ginkobiloba or Gensing and minerals like Zinc, or Seinite etc. So here is easy method to test the Vit. "C" in that drug.

PROCEEDURE: 

In the test , 1,2-diphenol-indophenol and metaphosphoric-acetic acid are used. first of all we are going to prepare both of these.

PREPARATION OF 1,2-diphenol-indophenol

Weigh 25mg of 1,2-diphenol-indolphenol in 100ml volumetric flask. add 25 ml of water and mix the weighed quantity. Now weigh 50mg of Sodium by carbonate and add in the mixture. add more 25ml of water and dissolve the reagents by continuous stirring by any mechanical means or  electromagnetic source.  and in last make the volume upto the marks using water.

PREPARATION OF Metaphosphoric Acetic-Acid

In a 100ml volumetric flask, Add 3ml of conc. phosphoric acid and 8ml of glacial acetic acid and makeup the volume upto the mark using distilled water. 

ASSAY OF VITAMIN "C"

Weigh accurately the product equivalent to 100mg of Vitamin C in 200ml volumetric flask. add 70ml of metaphosphoric acetic-acid in flask and sonicate for 30 minutes. Then makeup the volume upto the mark using distilled water. Mix the solution for 5 minutes and filter through whattman filter paper. or centrifuge some solution. take 4ml of the solution in a 100ml conical flask and add 5ml of metaphosphoric acetic acid. Now titrate with 1,2-diphenol-indophenol until rose pink color .  each ml of 1,2-diphenol-indophenol used is equivalent to 0.136mg of Vit.C.   Similar Posts :
    1. EDTA                                         2. Gentamicin Sulphate
   

Factors of Raw Material (Active)

Here is the list of factors for some raw material in B.P and U.S.P. By using these factors you can remove unwanted chemical groups from active and effective one. According to your label claim and raw material. I explain, let one has Lincomycin HCl and label claim for drug is only lincomycin then one should remove the HCl group or in other words, He should add so much quantity to manufacture a batch that the active Lincomycin should gave 100% assay when compared to B.P or U.S.P. Reference standard Lincomycin. For that reason here is the list of Raw Material factors that should be multiplied with the required quantity of raw material to fulfill the requirements of active present in raw material.
Sr. NoProduct NameMolecular WeightFactor
1Atorvastatin Calcium Trihydrate 1209.421.0843
Atorvastatin1115.34
2Azithromycin Dihydrate7851.0481
Azithromycin749
3Ciprofloxacin HCl Monohydrate 385.521.1646
Ciprofloxacin331.02
4Cetirizine Dihydrochloride 461.821.1878
Cetirizine370.38
5Cefixime Trihydrate 507.51.1192
Cefixime453.45
6Calcium Acetate 158.663.9479
Calcium40.07
7Cephradine Monohydrate 367.431.0516
Cephradine349.41
8Escitalopram Oxalate414.41.2774
Escitalopram324.39
9Esomeprazole Mg.Trihydrate 762.21.1137
Esomeprazole713.1
10Iron III Hydroxide Polymaltos Complex449.163.04
Elemental Iron147.75
11Levofloxacin Hemihydrate 370.381.0249
Levofloxacin 361.38
12Montelukast Sodium 608.171.0392
Montelukast 585.17
13Naproxen Sodium252.231.1003
Naproxen 229.23
14Pantoprazole Sodium Sesquihydrate432.41.1306
Pantoprazole382.4
15Lincomycin HCl461.011.134
Lincomycin406.51
16Gentamicin Sulphate Nlt 590 µg/mg1.6949
Gentamicin1000 µg/mg
17Thiamine HCl 337.31.1213
Thiamine300.8
18Pyridoxine HCl 205.61.2158
Pyridoxine 169.1
 

Gentamicin Sulfate

Gentamicin Sulfate

ABOUT:

Gentamicin Sulfate is the sulfate of a mixture of aminoglycoside substances having antibacterial activity produced by the growth of Micromonospora purpurea or Micromonospora echinospora.

PHYSICAL APPEARANCE:

Gentamicin Sulfate occurs as a white to light yellowish white powder. It is highly hygroscopic.

CHEMICAL FORMULA:

C21H43N5O7. xH2SO4 CHEMICAL STRUCTURE:
Gentamicin Sulfate
Gentamicin Sulfate

MOLECULAR WEIGHT:

477.60

IUPAC NAME:

(6R)-2-Amino-2,3,4,6-tetradeoxy-6-methylamino-6-methyl-α-D-erythrohexopyranosyl-(1→4)-[3-deoxy-4-C-methyl-3-methylamino-β-L-arabinopyranosyl-(1→6)]-2-deoxy-Dstreptamine sulfate

CONTENTS:

It contains not less than 590 mg (potency) and not more than 775 mg (potency) per mg, calculated on the dried basis. The potency of Gentamicin Sulfate is expressed as mass (potency) of gentamicin C1

SOLUBILITY:

  • Soluble in water.
  • Typically insoluble in ethanol. (96%)

IDENTIFICATION BY PPT. FORMATION:

Dissolve 50 mg of Gentamicin Sulfate in 5 mL of water, and add 0.5 mL of barium chloride TS: a white precipitate is formed.

COLOR OF SOLUTION:

Dissolve 1.0g of Gentamicin Sulfate in 10 mL of water, the solution is clear and colorless to pale yellow.

IDENTIFICATION BY THIN LAYER CHROMATOGRAPHY:

Dissolve 50 mg each of Gentamicin Sulfate and Gentamicin Sulfate Reference Standard in 10 mL of water, and use both of these solutions as the sample solution and standard solution. Perform the test with these solutions as directed under thin layer-Chromatography. Spot 20 µL of the sample solution and standard solution on a plate of silica gel for thin layer-Chromatography. Separately, shake a mixture of chloroform, ammonia solution and methanol in ration of (2:1:1) in a separator, and allow the mixture to stand for more than 1 hour. To 20 mL of the lower layer so obtained add 0.5 mL of methanol, and use this as the developing solvent. Develop the plate with the developing solvent to a distance of about 17cm in a developing container with a cover, having an opening of about 20 mm2, and without putting a filter paper in the container, and air-dry the plate. Allow the plate to stand in iodine vapors: three principal spots obtained from the sample solution are the same with the corresponding spots obtained from the standard solution in color tone and the Rf value, respectively.

pH:

The pH of a solution obtained by dissolving 400 mg of Gentamicin Sulfate in 10 mL of water is between 3.5 and 5.5

LOSS ON DRYING:

Not more than 18.0% when 0.15g of Gentamicin Sulfate at pressure not exceeding 0.67 kPa and temperature 110°C for 3 hours. Handle the sample avoiding absorption of moisture.

RESIDUE ON IGNITION:

Should be not more than 1.0% when 1.0 gram is ignited.

SPECIFIC OPTICAL ROTATION:

+107°   to   +121° When 100mg of Gentamicin Sulfate is dissolved in 10ml of water.

QUANTITATIVE ASSAY (BIO-ASSAY):

Perform the test according to the Cylinder-plate method as directed under Microbial Assay for Antibiotics according to the following conditions. Test organism Staphylococcus epidermidis ATCC Agar media for seed and base layer
  • Glucose 1.0 g
  • Peptone 6.0 g
  • Meat extract 1.5 g
  • Yeast extract 3.0 g
  • Sodium chloride 10.0 g
  • Agar 15.0 g
  • Water 1000 mL
Mix all the ingredients, and sterilize. Adjust the pH of the solution so that it will be 7.8 to 8.0 after sterilization. Agar medium for transferring test organisms. Use the medium Agar media for seed and base layer in Medium for other organisms under Agar media for transferring test organisms. Standard solutions Weigh accurately an amount of Gentamicin Sulfate Reference Standard, equivalent to about 25 mg (potency), dissolve in 0.1 mol/L phosphate buffer solution (pH 8.0) to make exactly 25 mL, and use this solution as the standard stock solution. Keep the standard stock solution at 15°C or lower, and use within 30 days. Take exactly a suitable amount of the standard stock solution before use, add 0.1 mol/L phosphate buffer solution (pH 8.0) to make solutions so that each mL contains 4 mg (potency) and 1 mg (potency), and use these solutions as the high concentration standard solution and the low concentration standard solution, respectively. Sample solutions Weigh accurately an amount of Gentamicin Sulfate, equivalent to about 25 mg (potency), and dissolve in 0.1 mol/L phosphate buffer solution (pH 8.0) to make exactly 25 mL. Take exactly a suitable amount of this solution, add 0.1 mol/L phosphate buffer solution (pH 8.0) to make solutions so that each mL contains 4 mg (potency) and 1 mg (potency), and use these solutions as the high concentration sample solution and the low concentration sample solution, respectively.

STORAGE CONDITIONS:

It should be stored in tight and air-free containers and should be keep away from moisture area.

REFERENCES:

Japan Pharmacopia (JP XVII) Official monographs Page 983. United State Pharmacopia (USP 41) Page 938.

Diclofenac Sodium

Diclofenac Sodium

DESCRIPTION:

Diclofenac Sodium is white or slightly yellowish, slightly hygroscopic, crystalline powder.

CHEMICAL FORMULA:

C14H10Cl2NNaO2

CHEMICAL STRUCTURE:

Diclofenac Sodium
Diclofenac Sodium

MOLECULAR WEIGHT:

318.1 Dalton

USE AS:

Cyclo-oxygenase inhibitor; analgesic; anti-inflammatory.

IUPAC NAME:

Sodium [2-[(2,6-dichlorophenyl)amino]phenyl]acetate.

CONTENTS:

It contains not less than 99.0% and not more than 101.0% of C14H10Cl2NNaO2.

SOLUBILITY:

  • Sparingly soluble in water.
  • Freely soluble in Methanol.
  • Soluble in ethanol.
  • Slightly Soluble in acetone.

MELTING POINT:

Determine the melting point of sample by using M.P instrument. It decomposes at 280°C.

IDENTIFICATION BY FTIR SPECTROPHOTOMETER:

Measure the FTIR spectra of sample and compare with standard.

IDENTIFICATION BY SODIUM REACTION:

Dissolve 60mg in 0.5mL of methanol and add 0.5 mL of water R. The solution gives reaction of sodium.

IDENTIFICATION BY COLOR OF SOLUTION:

Dissolve 1.25 gm in 25 mL methanol. And check its color & measure absorbance at 440 nm its absorbance should not be greater than 0.05

pH:

Dissolve 1.0 gm in Distilled water & dilute to 100ml and determine the pH. It should be in between 7.5 to 9.0.

LOSS ON DRYING:

Take 1.0gm of sample & dry in oven at 105-110oC for 3.0 hours. It should not be greater than 0.5%.

QUANTITATIVE ASSAY: (By Non-Aqueous TITRATION)

Dissolve 450 mg of Diclofenac Sodium in 25mL Glacial acetic acid. Add 2 drops of crystal violet indicator. Titrate with 0.1N Perchloric acid till change in color of indicator. If necessary, carry out blank titration. Each ml of 0.1N HClO4 is equivalent to 31.81 mg of C14H10Cl2NNaO2.

CALCULATIONS:

Calculate the Percentage of Diclofenac Sodium by using following Expression. %age assay = ((R x 31.81) /  (W-(100-X)) x 100 Where R = Reading at Burette (Vol. of 0.1N HClO4) W = Weight of sample taken X = Water contents

STORAGE CONDITION:

It should be packed in airtight containers. Containers should not be transparent to light.

REFERENCE:

British Pharmacopia 2016. Volume-I, Page 740

Pregabalin

Pregabalin
White Crystalline powder, Slightly hygroscopic. On dried basis, It contains 98.0% to 102.0% of Pregabalin.

Chemical Formula:

C8H17NO2

Chemical Structure

Pregabalin
Pregabalin

SOLUBILITY 

  • Soluble in Water
  • Slightly Soluble in Methanol
  • Very slightly soluble in ethanol
  • Practically insoluble in acetone, ethyl acetate, heptane and in methylene chloride

IDENTIFICATION BY FTIR SPECTROPHOTOMETER

Measure the FTIR spectra of sample and compare with standard.

IDENTIFICATION BY HPLC

The retention time of peak of Pregabalin in sample solution is similar to the retention time of peak of pregabalin in standard solution

APPEARANCE OF SOLUTION

Dissolve 0.5 grams in CO2 Free water and dilute 20ml with same solvent (solution S) The solution is clear and not more intensely colored than GY5

WATER CONTENTS

NMT 0.5%, determined on 0.200 gram

QUANTITATIVE ASSAY BY HPLC

  • Mobile Phase:
Mix 75 volumes of methanol and 25 volumes of a 6.805 grams/liter solution of potassium dihydrogen phosphate previously adjusted to pH 6.8.
  • Standard solution:
Dissolve 100 mg of pregabalin CRS in the mobile phase and dilute to 100ml with same solvent
  • Sample Solution:
Dissolve 100 mg of substance to examind in the mobile phase and dilute to 100ml with same solvent  

CHROMATOGRAPHIC SYSTEM

  • Mode    :   LC 100
  • Detector   :   UV 210 nm
  • Column   :   A stainless steel column 0.25 m ­x 4.6mm x 5 µm C18 packing; Octadecylsilanized silica gel (5µm particle diameter).
  • Column temperature :  Ambient
  • Flow rate   :   35 ml/min
  • CHROMATOGRAPHIC PROCEDURE

  • Inject 10µl of mobile phase (blank) and record the chromatograph
  • Inject 10µl of standard solution two times and record the chromatograph
  • Inject 10µl of sample solution and record the chromatograph
  • Inject 10µl of standard solution and record the chromatograph
  • Inject 10µl of mobile phase (blank) and record the chromatograph

CALCULATIONS

Calculate the Percentage of Pregabalin sample by using following formula  %age Assay = (At/As)× (Cs/Ct) × P Where At = Av. Area of the peaks in sample chromatograms As = Av. Area of the peaks in standard chromatograms Cs = Concentration (mg/ml) of standard Ct = Concentration (mg/ml) of sample P   =  Potency of reference standard  

Tranexamic Acid

Tranexamic Acid

Physical Appearance :

Tranexamic Acid occurs as white, crystals or crystalline powder. It belongs to antifibrinolytic family. Tranexamic Acid, when dried, contains not less than 98.0% and not more than 101.0% of tranexamic acid (C8H15NO2)

Structural formula:

 
Tranexamic Acid
Tranexamic Acid

Chemical Formula

(C8H15NO2).

Solubility:

It is freely soluble in water, and practically insoluble in ethanol (99.5).

Identification : BY FTIR

Determine the infrared absorption spectrum of Tranexamic Acid as directed in the potassium bromide disk method under Infrared Spectrophotometry, and compare the spectrum with the Reference Spectrum or the spectrum of Tranexamic Acid RS: both spectra exhibit similar intensities of absorption at the same wave numbers.

pH:

The pH of a solution prepared by dissolving 1.0 g of Tranexamic Acid in 20 mL of water is between 7.0 and 8.0.

Color of solution:

Dissolve 1.0 g of Tranexamic Acid in 10 mL of water: the solution is clear and colorless.

LOD: (LOSS ON DRYING)

Not more than 0.5% (1 g, for 2 hours).

Residue on ignition :

Not more than 0.1%

ASSAY : ( HPLC-Method)

Mobile Phase:

Dissolve 11.0 g of anhydrous sodium dihydrogen phosphate in 500 mL of water, and add 5 mL of triethylamine and 1.4 g of sodium lauryl sulfate. Adjust the pH to 2.5 with phosphoric acid or diluted phosphoric acid (1 in 10), add water to make 600 mL, and add 400 mL of methanol. Standard Preparation: Weigh accurately about 50 mg of Tranexamic Acid RS, previously dried, dissolve in water to make exactly 25 mL, and use this solution as the standard solution.

Sample Preparation:

Weigh accurately about 50 mg of Tranexamic Acid, previously dried, dissolve in water to make exactly 25 mL, and use this solution as the sample solution.

Chromatographic conditions:

Sample Volume: 20µL Detector: UV ʎmax=220nm Column: A stainless steel column 6.0 mm in inside diameter and 25 cm in length, packed with octadecylsilanized silica gel for liquid chromatography (5 mm in particle diameter). Column temperature: 25°C Flow rate: Adjust so that the retention time of tranexamic acid is about 20 minutes.

Calculations:

Contents of Tranexamic acid can be calculated by given formula %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)

Assay: (BY TITRATION) (non-aqueous )

Weigh accurately 10mg of tranexamic acid in a round 250ml conical flask and add 50ml of glacial acetic acid. Dissolve in magnetic stirrer. Now simply titrate it 0.1M perchloric acid. Each ml of 0.1M perchloric acid is equivalent to 15.72 mg of tranexamic acid.

Calculation:

Contents of Tranexamic acid can be calculated by given formula %age of tranexamic acid = (volume of 0.1M perchloric acid × 15.72) ÷ weight of sample taken.

ALTERNATIVE METHOD:(BY UV/vis Spectrophotometer)

STANDARD PREPARATION:

Weigh accurately about 50mg of Tranexamic acid of working standard in to 50ml volumetric flask and dilute it with distilled water. Take 1ml of this solution and dilute upto 100ml with the same solvent. SAMPLE PREPARATION: Weigh accurately about 50mg of Tranexamic acid of sample in to 50ml volumetric flask and dilute it with distilled water. Take 1ml of this solution and dilute upto 100ml with the same solvent. Take Reading at 210nm Contents of Tranexamic acid can be calculated by given formula %age of tranexamic acid= At/As × Cs/Ct × 100 At =  Absorbance Of  Tranexamic acid in Sample Solution. As =  Absorbance Of  Tranexamic acid in Standard Solution. Cs =  Concentration of standard solution (mg/ml) Ct =  Concentration of sample solution (mg/ml)

Alclometasone Dipropionate

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
Alclometasone dipropionate
Alclometasone dipropionate
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.