In this slide contains SAMPLING AND TESTING OF SKIN CARE PRODUCTS Presented by: BHANU TEJA (Department of pharmaceutical analysis).RIPER, anantapur

1. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 1
SAMPLING AND TESTING OF SKIN
CARE PRODUCTS
A Seminar as a part of curricular requirement
for I year M.Pharm Ⅱ semester
Presented by
R.Bhanu teja
(Reg. No.20L81S0707)
Pharmaceutical Analysis

2. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 2
• GENERAL REQUIREMENTS OF SAMPLING
• SAMPLING INSTRUMENTS
• SKIN CARE PRODUCTS
Contents

3. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 3
• Samples shall be taken in a protected place not exposed to damp air, dust or Soot.
• The sampling instrument shall be clean and dry.
• The samples, the material being sampled, the sampling instrument and the
containers for samples shall be protected from adventitious contamination.
• The samples shall be placed in clean and dry glass containers. The sample
containers shall be of a size such that they are almost completely filled by the
sample.
General requirements of samples

4. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 4
• Each container shall be sealed air-tight after filling and marked with full details of
sampling, batch or code number, name of manufacturer, and other important
particulars of the consignment.
• Sampling shall be done by a person agreed to between the purchaser and the supplier,
and in the presence of the purchaser or his representative and the supplier or his
representative.
• The sampling procedure at the point of manufacture shall consist essentially in
drawing samples of the finished product from the top, middle and bottom portions of
the process vessel immediately prior to packing.

5. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 5
For Powders
• For drawing samples of powders, a
sampling tube, commonly known as a
’ thief’ shall be used.
• This usually consists of two closely
fitting, concentric tubes with matching
slots that are closed by rotating the
tubes with respect to each other.
Sampling instruments

6. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 6

7. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 7
• For drawing samples a simple device DIPPER BOTTLE is used.
• consists of a small bottle and a two-hole stopper, one hole being
fitted with a short glass tube and the other with a glass tube slightly
longer than the depth of the vessel.
• To the longer tube is attached a stop-cock which is kept closed while
the bottle is lowered to the desired depth in a given process vessel.
• The stop-cock is then opened and, as the air escapes through the
longer tube, the product enters the bottle and fills it.
For homogenous liquids and thin
emulsions

8. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 8
Dipper bottle

9. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 9
• For drawing samples of emulsions, products, a sampling instrument similar to
powder thief may be used.
• However, the top end of the sampling tube should be connected to a suction device.
For Thick Emulsion’s Pastes and Gels

10. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 10
• consists of a tube fitted with a stopper at the lower end which can be closed by
means of an attached rod that extends above the upper end of the tube.
• With the stopper disengaged, the tube is lowered slowly into the vessel so that the
liquid enters it with minimum disturbance.
• When the bottom of the vessel has been reached, the lower end of the tube is closed
with the stopper and the tube is removed.
Bottom - valved sampling tube

11. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 11
Bottom- valved sampling tube

12. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 12

13. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 13
Skin powders shall be classified into two types as follows:
• a) Body powders shall include talcum powders, toilet powders, deodorant powders
and dusting powders.
These shall consist of a finely-powdered free flowing absorbent innocuous material
such as natural talc (hydrous silicate of magnesium with the formula 𝑀𝑔3𝑆𝑖2𝑂2,𝐻2𝑂)
and may contain small amounts of perfume and coloring matter, as well as other
ingredients consistent with the accepted practice in the cosmetic industry. The latter
may include materials having anti-per spirant and deodorant properties.
• b) Face powders shall essential y be similar to body powder described under a)
except that it shall be of finer particle size and free from grit.
Skin powders

14. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 14
• TEST FOR SOLUBILITY OF COLOURS
• DETERMINATION OF MATTER INSOLUBLE IN BOILING WATER
• DETERMINATION OF FINENESS
• DETERMINATION OF MOISTURE AND VOLATILE MATTER
• DETERMINATION OF pH OF AQUEOUS SUSPENSION
• TEST FOR HEAVY METALS
• DETERMINATION OF ARSENIC
Methods to evaluate skin powders

15. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 15
PROCEDURE 1:
• Take 1 g of the material and add 50 ml of water, boil for 15 minutes and filter.
• The filtrate shall be colorless or faintly colored.
PROCEDURE 2:
• Take 10 g of the material and add 50 ml of water, rectified spirit.
• Boil under reflux for 15 min and filter.
• The filtrate shall be colorless or faintly colored.
Test for solubility of colours

16. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 16
REAGENT
• Rectified Spirit
PROCEDURE
• Weigh accurately about 1g of the material and transfer to a 500mI beaker. If
necessary, wet the material with a little rectified spirit.
• Add to the beaker about 200ml of water and boil. Allow to settle and filter the
supernatant liquid through a Gooch crucible.
• Wash the residue in the beaker with water and transfer completely to the filter.
• Dry the residue in the crucible at 105±2°C to constant mass.
Determination of matter insoluble in
boiling water

17. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 17
REAGENT
• Denatured Spirit — Filtered.
PROCEDURE
• Place about 10g of the material, accurately weighed, in the specified IS Sieve and wash by means
of a slow stream of running tap water and finally with fine stream from a wash bottle until as
much material as would pass through the sieve has passed.
• In case the material is not easily wetted by water, the washing could be started with a slow stream
of filtered denatured spirit.
• Let the water drain from the sieve and then dry the sieve containing the residue on a stream bath.
• Transfer the residue onto a tared watch glass carefully and dry it to constant mass at 105±2°C .
Determination of fineness

18. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 18
PROCEDURE
• Weigh accurately about 5g of the material in a porcelain or glass dish
about 6 to 8 cm in diameter and about 2 to 4 cm in depth.
• Dry in an air oven at a temperature of 105 ± 2°C to constant mass
(within where ±5 mg).
Determination of moisture and
volatile matter

19. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 19
PROCEDURE
o Take 10 g of the material in a 150 ml beaker and add 90 ml of freshly boiled and
cooled water.
o Stir well to make a thorough suspension
o Determine the pH the suspension using a pH meter within 5 min of making the
suspension.
o In case of a material which does not wet, the pH shall be determined on the filtrate.
Determination of PH of aqueous
suspension

20. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 20
APPARATUS
• Nessler Cylinders — 50-ml capacity.
REAGENTS
• Dilute Hydrochloric Acid 5 N.
• Dilute Acetic Acid 1 N.
• Dilute Ammonium Hydroxide 5 N
• Hydrogen Sulphide Solution Standard.
Test for heavy metals

21. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 21
• Weigh about 2g of material in a crucible and heat on a hot plate and then in a
muffle furnace to ignite it at 600°C to constant mass.
• Add 3 ml of dilute hydrochloric acid, warm (wait till no more dissolution occurs)
and make up the volume to 100ml.
• Filter the solution.
• Transfer 25 ml of the filtrate into a Nessler cylinder.
• In the second Nessler’s cylinder, add 2 ml of dilute acetic acid, 1.0 ml of standard
lead solution and make up the volume with water to 25 ml.
Procedure

22. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 22
• Add 10 ml of hydrogen sulphide solution to each Nessler cylinder and make up the
volume with water to 50 ml.
• Mix and allow to stand for 10 min.
• Compare the color produced in the two Nessler’s cylinders. Blank determination
without samples are recommended to avoid errors arising out of reagents.

23. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 23
Requirements for skin powder

24. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 24
• The skin cream shall be in the form of a thick emulsion or unctuous mass with a
pleasant odor. It shall be white or pigmented or of uniform color.
Skin creams

25. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 25
• TEST FOR THERMAL STABILITY
• DETERMINATION OF pH
• DETERMINATION OF TOTAL FATTY SUBSTANCE CONTENT
• DETERMINATION OF RESIDUE
• TEST FOR HEAVY METALS
• DETERMINATION OF ARSENIC
Methods to evaluate skin cream

26. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 26
APPARATUS
• A humidity chamber/incubator controlled at 60 to 70 percent relative humidity and
45 ±1℃
• Clear glass bottles of around 30 ml capacity with plug and screw on cap for proper
closure.
Test for thermal stability

27. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 27
• With the help of spatula, insert the cream into glass bottle and tap it to settle to the
bottom.
• Fill up to two-third capacity of bottle and insert plug and tighten the cap. Keep the
filled bottle erect in side the incubator at 45 ±1℃ for 48 h.
• The sample shall be taken to have passed the test, if on removal from the incubator
shows no oil separation or any other phase separation
Procedure

28. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 28
APPARATUS
• A pH meter, preferably equipped with a glass electrode.
PROCEDURE
For Oil-in-Water Emulsion Creams
• Weigh accurately 5±0.01g of the cream in a 100ml beaker.
• Add 45ml of water and disperse the cream in it.
• Determine the pH of the suspension at 27°C using the pH meter.
Determination of PH

29. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 29
For Water-in-Oil Emulsion Creams
• Weigh 10 g of the cream to the nearest 0.1 g.
• Add 90 ml of rectified spirit previously adjusted to pH 6.5 to 7.0.
• Warm, if necessary to 45°C and stir thoroughly for 15 min.
• Filter the alcoholic layer through a filter paper and measure the pH of the filtrate
at 27°C using the pH meter.

30. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 30
REAGENTS
• Dilute Hydrochloric Acid — 1:1 (v/v).
• Petroleum Ether (60-80°C)
• Methyl Orange Indicator Solution
• Sodium Sulphate
Determination of total fatty substance
content

31. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 31
• Weigh accurately about 2g of the material into a conical flask, add 25ml of dilute
hydrochloric acid, fit a reflux condenser into the flask, and boil the contents until
the solution is perfectly clear.
• Pour the contents of the flask into a 300ml separating funnel and allow it to cool to
room temperature.
• Rinse the conical flask with 50 ml of petroleum ether in portions of 10ml.
• Pour the petroleum ether rinsing into the separating funnel, shake the separating
funnel well and leave until the layers separate.
• Separate out the aqueous phase and shake it out with 50 ml portions of petroleum
ether twice.
Procedure

32. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 32
• Combine all the ether extracts and wash them with water until free of acid (when
tested with methyl orange indicator solution).
• Filter the petroleum ether extracts through a filter paper containing sodium
sulphate into a conical flask which has been previously dried at a temperature of
90±2°C and then weighed.
• Wash the sodium sulphate on the filter with petroleum ether and combine the
washings with filtrate.
• Distil off the petroleum ether and dry the material remaining in the flask at a
temperature 90±2°C to constant mass.

33. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 33
PROCEDURE
• Weigh accurately about 5 g of the material in a weighed, clean and dry squat form
weighing bottle.
• Dry to constant mass at 105 ± 2°C.
• Cool in a desiccator and weigh.
Determination of residue

34. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 34
Requirements for skin creams

35. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 35
INDIAN STANDARDS
• IS 3959
• IS 5339
• IS 15153
• IS 6608
• IS 3958
References

36. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 36