USP is updating the General Chapter Zinc Oxide Testing by Alternate Method Determination of the monograph to include ion chromatography as a method for the assay. Zinc oxide is used in various skin care creams, drugs, and drug products. The ion chromatography analysis involves the separation of zinc followed by a post-column reaction using 4-(2-pyridylazo) resorcinol (PAR) reagent and subsequent detection at 530 nm wavelength.
Sample preparation consisted of 0.1868 g of sample dissolved in 10 mL 6 mol/L HCl and made up to 100 mL with ultrapure water.
This Raw material Specification & Analysis prescribes the requirements for Zinc Oxide Testing by Alternate Method, which is one of the components of a Capsule, tablet, and AX tablet.
It is applicable in the Material, Product Development, and Quality Assurance Department to confirm its physical & chemical specifications.
|1||Physical Form||Very fine, Amorphous Powder, free from gritty particles|
|2||Colour||White or Yellowish White|
|4||Solubility||Insoluble in water. Soluble in 0.01N Hydrochloric Acid|
|5||Alkalinity||Not more than 0.3ml of 0.1M Hydrochloric acid is required to change the color of the indicator.|
|6||Identification Test of Zinc Oxide||Yellow colour should produce which disappear on cooling.
White precipitate should produce.
|7||Contents of Zinc Oxide||99.0 to 100.5%|
Refer to the Incoming SOPs for sampling.
If the Zinc Oxide does not satisfy the specifications mentioned in 5.0 it will be rejected. In addition to the specifications, Zinc Oxide is also rejected due to the following reasons:
- If the receiving raw material is cross contaminated due to any reason.
- The material does not bear 75% of its stated shelf life at the time of receipt.
Zinc Oxide is received in glass bottle/plastic bottle to protect it from moisture and light.
Store in a well-closed container.
- Use gloves & mask during weighing and dispensing operation of Zinc Oxide.
- Keep the container of Zinc Oxide well closed immediately after use.
- Place the container of Zinc Oxide back to its specified area.
(A) Suitable Machinery/Equipment/Apparatus
|2||Glass Rod||Graduated Pipette 1 ml, 5 ml|
|5||Burette 25 ml|
|6||Titration Flask 250 ml|
(B) List Of Reagent/Chemical
|1||Conc. Hydrochloric Acid||5 ml|
|2||0.1 M Disodium Edetate||25 ml|
|3||Potassium Ferrocyanide TS||1 ml|
|4||Ammonia AmmoniumChloride Buffer pH7||10 ml|
|5||0.01 N Hydrochloric Acid||5 ml|
|6||Phenolphthalein TS||1 ml|
|7||Mordant Black II Solution||1 ml|
Test of Physical Form:
Check the sample and confirm its physical form; it should be Very fine, Amorphous Powder, free from gritty particles.
Test of Colour:
Confirm the colour of the material; it should be white or yellowish white.
Test of Odour:
Check the Odour of the sample; it should be odourless.
Test of Solubility:
- Check the solubility of the sample in water and in 0.01N Hydrochloric Acid;
- It should be insoluble in water and soluble in 0.01 N Hydrochloric Acid.
- Record the result of physical analysis on Quality Report.
Dissolve 10 g of the sample in 100 ml of distilled water. Take 10 ml from the resulting solution, add 0.1 ml of phenolphalein solution; Not more than 0.3ml of 0.1M Hydrochloric acid is required to change the color of the indicator.
Identification Test of Zinc Oxide:
a) Weigh accurately on analytical balance 2 g of the sample, put it in the test tube, and heat it on Bunsen burner; yellow colour should produce which disappear on cooling.
b) Weigh accurately on analytical balance 100 mg of the sample, put it in the test tube, add 2 ml of 0.01 N hydrochloric acid, 1 ml of potassium ferrocyanide TS; white precipitate should produce.
Contents of Zinc Oxide:
Weigh accurately on analytical balance 100 mg of the powdered sample of Zinc Oxide, put it in 250 ml titration flask, add 4 ml of conc. hydrochloric acid, 100 ml of distilled water, and 10 ml of ammonia ammonium chloride buffer solution pH 10.
Titrate step 220.127.116.11.1 with the help of 25ml burette with 0.1 M Disodium Edetate using Mordant Black II Solution as an indicator.
a) Volume of 0.1 M Disodium Edetate solution used for sample = A
b) Record the reading.
Calculate the contents of Zinc Oxide as follows:
Factor: Each ml of 0.1 M Disodium Edetate solution is equivalent to 8.14 mg of Zinc Oxide.
8.14 x A
—————————————- X 100 = B
Limit: The contents of Zinc Oxide should be between 99-100.5%.
Note. Incase of any non- conformance observed during Inspection and testing , Please Follow Quality System Procedure for Control of Non-Conforming Product. (CCL-CQP-010)
Total No. of Worker/Officer and Time.
Officer = 2 Worker = 3 Total Time consumed = 1:00 Hours
RESPONSIBILITIES AND AUTHORITIES
- Product Development Manager
- Product Development Officer
- Quality Control Manager
- Quality Assurance Officer
- Quality Assurance Assistant
- Quality Assurance Attendant
COMPANY QUALITY FORMS:
• Quality Report