Standard test procedure of raw Material Iron sucrose

1.0 OBJECTIVE
1.1 To lay down a procedure for Analysis of Iron sucrose.

2.0 SCOPE
2.1 This procedure is applicable to the Analysis of Iron sucrose in QC lab

3.0 RESPONSIBILITY
3.1 Q.C- Chemist

4.0 ACCOUNTABILITY
4.1 Head-Quality Assurance

5.0 Definition: – Iron contains NLT 4.8 % and NMT 6.0 % of iron and sucrose79.0 % to 91.0 % of Sucrose.

6.0 Description: – Reddish brown to dark brown powder.

7.0 Solubility: – Freely soluble in water.

8.0 Identification: –
(A) Iron: – To 50 mg. sample add 17.5 ml of water and 5 ml of hydrochloric acid mix and heat for 5 minutes in a boiling water bath. Cool and dropwise 13.5 N ammonium hydroxide until no further precipitation of ferric hydroxide occurs and filter wash the precipitate with water to remove excess ammonium hydroxide, dissolve the precipitate in Aluminium volume of 2 N hydrochloric acid, and add sufficient water to make a volume of 20 ml .to 3 ml of the solution so obtained add 1 ml of potassium thiocyanate the resulting solution is red. To 1 ml of solution add 5 ml of amyl alcohol or ethyl ether shake and allow to stand the organic layer is pink. To a separate 1 ml aliquot of solution add 2 ml of mercuric chloride the red colour is discharged iron (iii).

(B) Sucrose: – In the assay the principal peak in the chromatogram obtained with the test solution corresponds to the peak in the chromatogram obtained with the reference solution.

9.0 pH: -Sample solution: – 2 % w/v iron solution.
Acceptance criteria: – 10.5 to 11.1

10.0 Specific gravity: –
Sample solution: – 2.0 % w/v iron solution
Acceptance criteria: -1.135 to 1.165

11.0 Alkalinity: –
Sample solution: – 2.0 % w/v iron solution
Acceptance criteria: -0.5-0.8 ml of 0.1N hydrochloric acid consumed /ml.

12.0 Chloride contain: –
Sample solution: – 2.0 % w/v iron solution between 0.012 % – 0.025 %
As solid: – between 0.03 % – 0.08 %

13.0 Loss on drying: – not more than 5.0 per cent determine on 1.0 gm. by drying in an oven at 1050 at 1 hour.

14.0 Bacterial endotoxins: – Not more than 3.7 USP Endotoxin per mg. of iron sucrose as per
14.1 Materials Required:
14.1.1 LAL Reagent Water, Control Standard Endotoxin, LAL Reagent, Depyrogenated Micro tips (100 μl &1000 μl), Glass test tube (Depyrogenated), Sample to be tested.

14.2 Equipment Required:
14.2.1 Micro pipettes (1000 μl &100 μl), Vortex Mixer, Heating block

14.3 Procedure for Testing:

14.4 Preparation of Maximum valid dilution:

14.4.1 When the endotoxin limit in the substance or preparation being examined is specified in terms of

weight or units of active drug, the MVD may be calculated by the following formula:

– ———– Endotoxin Limit (in EU/ ml /mg) X Potency of product

MVD = ———————————————————————

– —————————-Labeled sensitivity of lysate in EU /ml (l)

– Where Potency =Concentration of the drug in mg / ml or unit /ml

14.4.2 When the endotoxin limit in the sample preparation is specified in terms of volume,

the MVD may be calculated by the following formula.

15.0 Microbial limit test: –

– ———————– Endotoxin Limit (EU/ml)

MVD = —————————————————–

– ————————– Labeled sensitivity of lysate in EU/ml (l)

15.0 Microbial limit test: – Microbial limit test

16.00Assay: –

Composition: –

Each 5 ml contains:

Ferric hydroxide in complex with sucrose

Eq. to elemental iron 100 mg.

16.0 Assay: –

Method of Iron: – Determine by atomic absorption spectrophotometry.
Transfer about 350mg of ferrous ammonium sulfate, accurately weighed, to a 100ml volumetric flask add water to dissolve,

dilute with water to volume and mix to obtain a solution having a concentration of about 50µg of iron per ml.
Transfer2.64g of calcium chloride to a 100ml volumetric flask add 500ml of water, and swirl to dissolve

add 5.0ml to hydrochloride acid and dilute with water to volume.
To separate 50ml volumetric flasks transfer 2.0 ,4.0 ,6.0 ,8.0, and 10.0ml of iron stock solution dilute

each flask with calcium chloride solution to volume and mix to obtain standard preparations having

known concentration of about 2.0 ,4.0 ,6.0 ,8.0 and 10.0µg of iron per ml.

Sample preparation: -Take sample equivalent about 2.0 ml injection of 100 ml volumetric flask add 5 ml of hydrochloric acid until the solution turns yellow dilute with the calcium chloride further dilution 2.0 ml to 100 ml volumetric flask with calcium chloride.

Chromatographic condition: -Wavelength-248.3 nm with the suitable atomic absorption spectrophotometry.

Assay: –
Method of sucrose: – Determine by liquid chromatography.
Mobile phase: Acetonitrile: water. (79 : 21)
Standard preparations— Dissolve an accurately weighed quantity of USP Sucrose RS in water, and quantitatively dilute with water to obtain solutions having known concentrations of about 13, 16, 18, 21, and 23 mg of sucrose per ml.

Sample preparation: -Transfer about 1.875 g of Injection, accurately weighed, into a 25-mL flask, add 1.25 mL of water, and mix. Add 1.25 mL of a monobasic sodium phosphate solution, prepared by dissolving 30 g in 50 mL, and mix. Allow the resulting solution to stand for 10 minutes to precipitate the colloidal ferric hydroxide. Dilute with water to volume, and mix. Centrifuge this solution at 3000 rpm for 15 minutes. Pass the resulting solution through a filter, discarding the first 2 mL of the filtrate.

Chromatographic condition: -The liquid chromatograph is equipped with a column compartment and a refractive index detector each maintained at a controlled temperature between 20 and 25 (±2) and a 4-mm × 25-cm column that contains packing L8. The flow rate is about 2.0 mL per minute. Chromatograph the Standard preparations, and measure the peak areas as directed for Procedure. The correlation coefficient obtained from the linear regression of the Standard preparations is not less than 0.998. [NOTE—The retention time for sucrose is about 8 minutes.

17.0 ABBREVIATION

Sr. No. Abbreviation used Full form of abbreviation used
1.0 STP Standard Testing Procedure
2.0 QA Quality assurance
3.0 STD Standard
4.0 SPL Sample
5.0 NM Nano Meter

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