आपक अवल कन ह त तन नमल तत र त षवत स स स ल न ह : Mehendi (Henna) Paste in Shape of Cone and other Allied Packaging Specification (New Standard)

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1 र त षवत स स रलजख रजषण स ञ पन स द भ ददन क प स ड /19/ /05/2016 रस धन तकन क सम तत: प स ड 19 र ष त रस धन तकन क सम तत, प स ड 19 एव इसक सभ उपसम ततय क स त सस य ह सय, ह सय / आपक अवल कन ह त तन नमल तत र त षवत स स स ल न ह : मस द स य प स ड /19/10319 व षय Mehendi (Henna) Paste in Shape of Cone and other Allied Packaging Specification (New Standard) क पय इस स स क अवल कन कर अपन स ततय यह तत त ह ए भ क यदस अ तत यह : र त षवत नक स स र र य नक क प रक म त ह ए त इस पर अ ल करन आपक यवस य अवव क र त र य कद न इय आ सकत ह स मतत जननज क ततम तत : 19/06/2016 स तत क पय स ल न र प अध र क भ ह त - ध यव स, रतत उपररमल तत भवस य ए क भटन गर वञ तनक 'ऐफ एव र त ) प स ड ) ई- ल :pcd19@bis.gov.in, pcd@bis.gov.in,

2 PRELIMINARY DRAFT Document Dispatch Advice Ref. Date PCD/19/ /05/2016 Technical Committee: Cosmetics Sectional Committee, PCD 19 and its Subcommittees Addressed to: All Members of Cosmetics Sectional Committee, PCD 19 and its Subcommittees Dear Sir(s)/Madam(s), Please find enclosed the following Proposed Draft Indian Standard: Doc No. PCD/19/ Title Mehendi (Henna) Paste in Shape of Cone and other Allied Packaging Specification (New Standard) Last date for comments: 19/05/2016 Comments if any; may please be made in the format as given overleaf and mailed to the undersigned at our address. Thanking you, Yours faithfully, Encl.: As above. A.K. Bhatnagar Sc. F & Head (PCD) pcd19@bis.gov.in; pcd@bis.gov.in

3 FORMAT FOR SENDING COMMENTS ON BIS DOCUMENTS (Please use A4 size sheet of paper only and type within fields indicated. Comments on each clauses/sub-clauses/table/fig. etc to be started in a fresh box. Information in Column 5 should include reasons for the comments and suggestions for modified wording of the clauses should be typed in Column 6 when the existing text is found not acceptable. Adherence to this format facilitates Secretariat s work) Doc. No.: PCD/19/ TITLE: Mehendi (Henna) Paste in Shape of Cone and other Allied Packaging Specification (New Standard) LAST DATE OF COMMENTS: 19/06/2016 NAME OF THE COMMENTATOR/ORGANIZATION: Sl. No. (1) Clause/Sub-clause/ Para/Table/Fig. No. commented (2) Commentator/ Organization/ Abbreviation (3) Type of Comments (General/Editorial/ Technical) (4) Justification (5) Proposed Change (6)

4 For BIS Use Only Doc: PCD/19/10319 May 2016 BUREAU OF INDIAN STANDARDS Proposed Draft Indian Standard MEHENDI (HENNA) PASTE IN SHAPE OF CONE AND OTHER ALLIED PACKAGING - SPECIFICATION Last date for receipt of comment is: 19/06/2016 ICS Working Draft prepared by Panel under Convenership of Shri M. B. Desai, Hygienic Research Institute Pvt. Ltd. FOREWORD (Formal clauses will be added later) Henna (Mehendi), Lawsonia Inermis Linn has been known as natural source of dye having medicinal properties. After dilution with water, Henna powder is used as paste for skin decorations, tattooing and hair dying. Upon drying, the paste imparts orange, dark Brown/ black coloration to skin. In order to help the users, henna paste is supplied in the conical packing to facilitate several types of designs on the hands & other parts of body as it has better design maneuverability. Many commercial products available in the market lose its staining power on storage especially ones packed in cones. Destabilized paste of henna cones when used does not give any coloration. To increase the staining power and market value, some products are sold with chemicals like dyes & pigments which are allergic e.g. para phenylenediamine etc. The henna paste in the form of cones are manufactured as micro business activity in small households, by road side vendors and small shops, which make paste in small lots & immediately fill in plastic or metalized film and sell on the spot. These cones do not have a shelf life of more than one week. Here ph and water quality used to manufacture henna paste play an important role in stability and color impartation.

5 1. SCOPE The standard prescribes the requirements and the methods for sampling and test for Mehendi (Henna) paste in shape of cone and other allied packaging. 2. REFERENCES The following standards contain provisions, which through reference in this text, constitute provisions of this standard. At the time of publication, the editions indicated were valid. All standards are subject to revision and parties to agreements based on this standard are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below: IS No. Title 1070 : 1992 Reagent grade water (third revision) 3958 : 1984 Methods of sampling cosmetics (first revision) 4011 : 1997 Methods of test for safety evaluation of cosmetics (second revision) 4707 Part 1) : 2009) Classification of cosmetic raw materials and adjuncts: Part1: Dyes, colours and pigments (second revision) 4707 (Part 2) : 2009 Classification of cosmetic raw materials and adjuncts: Part 2: List of raw materials generally not recognized as safe for use in cosmetics (second revision) : 2005 Test Method for Microbiological Estimation 3. REQUIREMENTS 3.1 Description The Mehendi (Henna) Paste is a stable paste of henna powder in water which imparts colour stains on skin/hair without addition of any chemical dyes. 4. INGREDIENTS 4.1 The Mehendi (Henna) Paste is formed by soaking henna powder in water. Other natural ingredients like powders of Aamla, Reetha, Bhangraj, Jatamasi etc. can also be mixed with henna powder. 4.2 It may contain small quantities of essential oils, preservative, citric acid and lemon juice etc. for colour enhancement and ph maintenance.

6 4.3 Unless otherwise specified, all the raw materials; used in the manufacture of henna paste shall conform to the requirements prescribed in the relevant Indian Standards where such Standard exists. 4.4 All ingredients of henna paste shall comply with the provisions of IS 4707 (Part 1) and IS 4707 (Part 2) subject to the provisions of the Drugs and Cosmetics Act, 1940 and rules framed there under. 4.5 The material shall comply with the requirements given in Table 1 Table 1 Requirement for Mehendi (Henna) Paste (Clause 4.5) Sl No. Characteristic Requirement Method of Test, Ref to Annex Indian Standard (1) (2) (3) (4) (5) i) ph 3.0 to 4.5 A -- ii) Loss on Drying 65 to 75 % B -- iii) Lawsone Pigment Content NLT 0.75 % C or D -- iv) Determination of absence of chemical dyes & pigment v) Heavy metals as lead (Pb) 2), parts per million, Max vi) vii) Arsenic (as As 2 O 3 ) 2), parts per million, Max Microbial count a) Total viable count, cfu/g, Max b) Gram negative pathogens/g 4.6. Additional requirements for Eco-Mark General Requirements To pass the test E F -- 2 G Absent -- IS 14648: The product shall conform to the requirements to the requirements for quality, safety and performance prescribed under 4.1 to All the ingredients that go into formulation of cosmetics shall comply with the provisions for IS 4707 (Part 1) The material used for product packaging shall be recyclable, reusable or biodegradable The product package shall display a list of ingredients in descending order of quantity present The product shall not be manufactured from any carcinogenic ingredients.

7 The manufacturer shall produce to BIS the environmental consent clearance from the concerned State Pollution Control Board as per the provisions of Water (Prevention & Control of Pollution) Act, 1981 along with the authorization, if required under Environment (Protection) Act, 1986 and Rules made there under while applying for ECO-Mark. Additionally provision of the Drugs and Cosmetics Act, 1940 and the Rules there under shall also be complied with The product package shall be suitably marked that ECO-Mark label is applicable only to the contents, if the product package is not separately covered under the ECO-Mark scheme The product package shall display in brief the criteria based on which the product has been labeled environment friendly The material for product packaging shall meet the parameters evolved under the scheme of labeling environment friendly packaging/packaging materials Specific Requirement Product shall be dermatologically safe when tested as prescribed in IS Heavy metals calculated as lead (Pb) and arsenic as (A S 2O 3 ) shall not exceed 20 and 2 ppm, respectively when tested by the respective method prescribed in Indian Standards. 5. PACKING & MARKING 5.1 Packing The Mehendi (Henna) Paste can be packed in plastic / metalized films drawn into a cone or any suitable plastic or multilayer packing to give protection during its shelf life and should be suitably labeled. 5.2 Storage The material shall be stored in a dark place away from heat and direct sunlight. 5.3 Marking Each container (cone/jar/bottle/etc) and package containing this in a carton / box shall be marked with following information: a) Name of material, b) Name & address of the manufacturer, c) Net quantity, d) Lot No. / B. No. pertaining to manufacture of bulk, e) Best use before (Month & Year to be declared by manufacturer), f) Any other information required by statutory bodies, g) Additional instructions for use, can be provided in accompanying leaflet if possible.

8 h) Cautions: Do not use in the area of the eyes. Do not use on cut or abraded scalp. 5.4 BIS Certification Marking The product may also be marked with the Standard Mark The use of the Standard Mark is governed by the provisions of the Bureau of Indian Standards Act, 1986 and the Rules and Regulations made there under. The details of conditions under which the license for the use of the Standard Mark may be granted to manufacturers or producers may be obtained from the Bureau of Indian Standards. 6. SAPMLING 6.1 Representative samples of the material shall be drawn as prescribed in IS Test for all characteristics shall be carried out on the composite sample. 6.3 The material shall be taken to have confined to the specification if the composite sample passes all the tests. 7. QUALITY OF REAGENTS Unless otherwise specified, pure chemicals and distilled water (see IS 1070) shall be employed in tests. Note: Pure chemicals shall mean chemicals that do not contain impurities which affect the results of analysis. A-1 Apparatus ANNEX A [Table 1, Item (i)] DETERMINATION OF ph A-1.1 ph meter- preferably equipped with glass electrode. A-2 Procedure A-2.1 Take 50 ml of the henna paste and determine its ph at C using ph meter. ANNEX B [Table 1, Item (ii)]

9 B-1 OUTLINE OF THE METHOD DETERMINATION OF LOSS ON DRYING This method determines loss on drying which is the loss in weight in % w/w resulting from water and volatile matter of any kind that can be driven off under specified conditions. The test vg carried out on a well mixed sample of the substance B-2 Apparatus Drying oven. B-3 Procedure B-3.1 Weigh a glass stoppered, shallow weighing bottle that has been previously dried under the same condition to be employed in the determination & cooled in desiccators. Note down the weight W1. B-3.2 Transfer 1g of sample to the bottle or the quantity of the sample specified in the individual monograph, cover it & accurately weigh the bottle and the contents. Note down the weight as W2. Distribute the sample as evenly as practicable by gentle sidewise shaking to a depth not exceeding 10 mm. B-3.3 Place the loaded bottle in the drying chamber (oven or desiccators) as directed in the monograph, remove the stopper and leave it also in the chamber. B-3.4 Dry the sample to constant weight means that the drying process should be continued until the results of two consecutive weighings do not differ by more than 0.5 mg, second weighing being made after an additional hour of drying under the prescribed conditions or for the specified time and at the temperature as specified in the monograph. B-3.5 After drying is completed, open the drying chamber, close the bottle promptly and allow it to cool to room temperature (where applicable) in a desiccators before weighing. Weigh the bottle and the contents.w3. Calculate the loss on Drying from the equation : Loss in weight % Loss on drying = x 100 Weight of sample taken W3 W2 % Loss on drying = x 100 W2 - W1

10 ANNEX C [Table 1, Item (iii)] DETERMINATION OF LAWSONE PIGMENT CONTENT C-1 OUTLINE OF METHOD The pigment is extracted and the Lawsone content is determined by comparing the observed optical density (measured colorimetrically) with a calibration curve, relating optical density to various concentrates of 2-hydroxy, 1-4-napthoquinone. C-2 APPARATUS Spectrophotometer or photoelectric Colorimeter with a filer of 490 nm. C-3 REAGENTS Sodium Bicarbonate Solution 5 % (m/v) Hydroxy, 1-4-napthoquinone C-4 PROCEDURE C-4.1 Preparation of Standard Calibration Curve Prepare standard 0.1 % stock solution of 2-hydroxy, 1-4-napthoquinone (C 10 H 6 O 3 ) by dissolving it in sodium bicarbonate solution, 5% (m/v). Pipette 0 ml (Blank), 1 ml, 2 ml, 3 ml, 4 ml and 5 ml of standard 0.1 % stock solution in 100 ml volumetric flasks and dilute with sodium bicarbonate solution 5 %, (m/v) up to the mark, Measure the optical density of these solutions having varying concentration from 0.0, 10, 20 to 50 ppm of 2-hydroxy, 1-4-napthoquinone, at 490 nm with a spectrophotometer and construct a calibration curve. The stock solution should not be stored for more than one month. C-4.2 Weigh 2.0 g of the prepared sample. Transfer it to a 100 ml volumetric flask. Add sodium bicarbonate solution, 5 % (m/v) and make up the volume to mark. Shake the contents of the flask every half an hour or so for about 8 h. Allow to settle overnight. Thereafter filer the solution through a filter paper and reject the first few milliliters. Take 10 ml of the filtrate in a 25 ml volumetric flask and dilute with 5 % sodium bicarbonate solution up to the mark. Measure the optical density of this solution with a spectrophotometer at 490 nm. C-5 Calculation:

11 Refer to the calibration curve and determine the percent Lawsone content of the sample from the curve. ANNEX D [Table 1, Item (iii)] DETERMINATION OF LAWSONE PIGMENT, BY HPLC D-1 CHROMATOGRAPHIC CONDITIONS Column: Microsorb - MV C X 4.6mm Mobile phase: Methanol :Water with 1% Ortho Phosphoric acid,(50:50) Wavelength: 286 nm Flow rate: 1 ml /min Temperature: Ambient D-2 SAMPLE PREPARATION Weigh 2.0 g of sample. Transfer it to a 100 ml volumetric flask. Add 5% (m/v) Solution of sodium bicarbonate and make up the volume to mark.shake the contents of the flask every half an hour or so for about 8 hours. Allow to settle overnight, there-after filter the solution through a filter paper and reject the first few milliliter. Take 10 ml of the filtrate in a 25 ml volumetric flask and dilute with distilled water up to the mark. Use this solution for HPLC. D-3 STANDARD PREPARATION Take weight g/100 ml of Standard 2-hydroxy-1 4-naphthoquinone and prepared same as described under sample preparation. D-4 STABILITY AND STORAGE PREPARATION The standard and sample are stable when stored in glass volumetric flask and are refrigerated. D-5 CALCULATIONS Area of sample x conc. of Std. x Purity (95%)_ Area of Std. x conc. of sample ANNEX E [Table 1, Item (iv)] DETERMINATION OF ABSENCE OF CHEMICAL DYES & PIGMENT

12 E-1 OUTLINE OF METHOD To detect contamination of chemical dyes/ synthetic pigments if any, the method for Thin Layer Chromatography shall be run. E-2 APPARATUS E-2.1 Weighing balance, E-2.2 TLC Plates precoated silica gel 60 F 0.2 mm thickness, E-2.3 TLC apparatus / beakers 250 ml (narrow), E-2.4 Iodine chamber, E-2.5 Test tubes with stoppers, E-2.6 Pipette, E-2.7 Syringe, E-2.8 Silicone Wax, E-3 REAGENTS E-3.1 Benzene, AR grade E-3.2 Ethyl Acetate, AR grade E-3.3 Methanol, AR grade E-3.4 Sodium Sulphite, AR grade E-3.5 Standards Chemical/synthetic dye ingredients like para Phenylene Diamine, Resorcinol, E-3.6 Basic Red, Basic Yellow, etc. E-3.7 Test sample 1 g of Henna paste sample being tested E-4 PREPARATION OF SOLUTION E-4.1 Mobile phase Benzene AR, Ethyl Acetate AR (3: 7 v/v) Take the solvents benzene AR and ethyl acetate AR in 3: 7 v/v, mix well and keep stoppered. E-4.2 Sample Solutions: Weigh accurately 1 g of sample being tested. Add a small quantity of sodium sulphite, add 4 ml of methanol AR and mix well. Use this solution for spotting. E-4.3 Standard Solutions: Weigh quantity nearly sufficient of the standard dye/ intermediates like para Phenylene diamine, Resorcinol, Basic Red, Basic Yellow, etc. Add sodium sulphite and dissolve in 5 ml of methanol AR. E-5 PROCEDURE E-5.1 Pour ml of mobile phase into the 250 ml narrow beaker (developing chamber) and cover with a suitable petri dish using silicone wax as a sealant.

13 E-5.2 Spot1µl of the test solution slowly on the TLC plate. Similarly spot the standard solutions as mentioned above. Allow spots to dry and develop in the developing chamber. E-5.3 Remove the TLC plate when the mobile phase reaches 0.5 cm away from the end of the TLC plate. E-5.4 Allow the plate to dry completely and develop the spots in an Iodine chamber. E-5.5 Observe and compare the Rf values, colour, shape and size of the sample spots versus the standard spots to identify and determine the absence of chemical/synthetic dye ingredients/pigments in sample. F-1 OUTLINE OF THE METHOD ANNEX F [Table 1, Item (v)] TEST FOR LEAD The color produced with hydrogen Sulphide solution is matched against that obtained with standard lead solution. F-2 APPARATUS F-2.1 Nessler Cylinders 50 ml capacity. F -3 REAGENTS F-3.1 Dilute Hydrochloric Acid Approximately 5 N F-3.2 Dilute Acetic Acid Approximately 1 N F-3.3 Dilute Ammonium Hydroxide Approximately 5 N F-3.4 Hydrogen Sulphide Solution Standard F-3.5 Standard Lead Solution Dissolve g of lead nitrate in water and make up the solution to 1000 ml. Pipette out 10 ml of the solution and dilute again to 1000 ml with water. One milliliter of this solution contain 0.01 mg of lead (as Pb) F-4 PROCEDURE

14 Weigh about g of material in crucible and heat on a hot plate and then in a muffle furnace to ignite it at 600 o C to constant mass. Add 3 ml of dilute hydrochloric acid, warm (wait till no more dissolution occurs) and make up the volume to 100 ml. Filter the solution. Transfer 25 ml of the filtrate into a Nessler s 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. 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 colour produced in the two Nessler s cylinders. Blank determination without samples are recommended to avoid errors arising out of reagents. F-5 RESULTS The sample may be taken to have passed the test, if the colour developed in the sample solution is less than that of standard solution. G-1 OUTLINE OF THE METHOD ANNEX G [Table 1, Item (vi)] TEST FOR ARSENIC Arsenic present in a solution of the material is reduced to arsine, which is made to react with mercuric bromide paper. The stain produced is compared with a standard stain. G-2 REAGENTS G-2.1 Mixed Acid Dilute one volume of concentrated Sulphuric acid with four volumes of water. Add 10 g of sodium chloride for each 100 ml of the solution. G-2.2 Ferric Ammonium Sulphate Solution Dissolve 64 g of ferric ammonium Sulphate in water containing 10 ml of mixed acid and make up to one liter. G-2.3 Concentrated Hydrochloric Acid (see IS 265) G-2.4 Stannous Chloride Solution Dissolve 80 g of stannous chloride (SnCl 2.2H 2 O) in 100 ml of water containing 5 ml of concentrated hydrochloric acid. G-3 PROCEDURE Carry out the test as prescribed in IS 2088, adding into the Gutzeit bottle, 2 ml of ferric ammonium Sulphate solution, 0.5 ml of stannous chloride solution and 25 ml of sample solution as prepared in F-4

15 For comparison, prepare a stain using mg of arsenic trioxide.