Synthetic Organic Colorants in Paper and Paperboard

The Commissioner of Foods and Drugs has evaluated data submitted by Synthetic Organic Chemical Manufacturers Association of the United States, 261 Madison Avenue, New York, N.Y. 10016, and other relevant information, and concludes that a food additive regulation should be proposed that would provide for the safe use under certain conditions of synthetic organic colorants in foodpackaging paper and paperboard. Accordingly, pursuant to the provisions of the Federal Food, Drug, and Cosmetic Act (sec. 409(d), 72 Stat. 1787; 21 U.S.C. 348(d)) and under the authority delegated to the Commissioner by the Secretary of Health, Education, and Welfare (21 CFR 2.120), it is proposed that Part 121 be amended by adding to Subpart F a new section as follows: § 121. Synthetic organic colorants in paper and paperboard.

(a) Conditions of use. Synthetic organic colorants may be safely used to impart color to food-packaging paper and paperboard otherwise complying with regulations in this Subpart F if one of the conditions set forth in subparagraphs (1) through (4) of this paragraph plus the conditions set forth in subparagraph (5) of this paragraph are met:

(1) There is a functional barrier between the colored paper or paperboard and the food.

(2) The colorant is listed as a color additive for food use by a regulation in Part 8 of this chapter.

(3) The colored paper or paperboard is used or intended for use in contact with a dry food the surface of which contains no free fat or oil.

(4) The colorant is applied to the paper or paperboard only prior to the sheetforming operation, the colored paper or paperboard is used or intended for use in contact with food containing not over 2 weight percent of free drainable liquid, and it passes the extraction and discoloration tests described in paragraph (b) of this section.

(5) The colorant contains, if at all, only useful adjuvants that:

(i) Are permitted to be added directly to food by a regulation in Subpart D of this part; or

(ii) Are otherwise permitted in the manufacture of paper and paperboard by a regulation in this Subpart F and are so used as to meet any limitations prescribed by such regulation.

Failure to meet the appropriate conditions prescribed by this paragraph will cause the colorant to be deemed a food additive for which no regulation exists. (b) Tests. The tests referred to in paragraph (a)(4) of this section are as follows:

(1) Food-simulating solvents. Food-simulating solvents are chosen from the following table:

Types of food

I. Nonacid, moist products; may contain salt or sugar or both (pH above 5.0).

Water.1

Solvent

II. Acidic, moist products; may contain salt or Water,' citric acid." sugar or both, and including oil-in-water emulsions of high or low fat content.

III. Moist, acid or nonacid products containing free
oil or fat; may contain salt, and including
water-in-oil emulsions of high or low fat
content.

IV. Dairy products and modifications_
V. Low-moisture fats and oils___.

VI. Bakery products, except dry foods_-_.

VII. Dry solids with the surface containing no free fat or oil.

VIII. Dry solids with the surface containing free fat

oil.

XI. Fruits and vegetables, raw.

1 Water either distilled or demineralized.

Water,' citric acid, lard oil.3

Water,' lard oil.'
Lard oil.

Water,' lard oil.
No end test required.

Lard oil.3

Water.1

2 Citric acid solution-20 percent sucrose solution containing 1 percent citric acid adjusted to pH 3.5.

3 Lard oil-an industrial grade of lard oil is satisfactory. Omit unless food is acid.

(2) Drainable liquids in foods. The test for drainable liquids in food is as follows: A 100-gram sample of the food in question is placed on a 5-inch diameter, U.S. standard sieve No. 8, tilted approximately 30° from the horizontal and drained for 2 minutes at ambient temperatures of not less than 65° F. The weight of the extracted liquid shall not exceed more than 2 weight percent of the original sample.

(3) Color transfer. The test for color transfer from treated paper and paper board ("sandwich test") involves visual comparison against a standard of a moist filter paper held in contact with the colored paper under test for a standard period of time.

(i) Equipment. (a) Color transfer standard: Color standard No. 4 of the "Official chart for Measuring Transference of Color of the American Association of Textile Chemists and Colorists."

(b) Glass-fiber filter paper.

(c) Aluminum foil.

(d) Tweezers.

(e) Appropriate solvents simulating the foods to be contacted by the paper or paperboard under test.

(f) Approximately 1-inch squares of the paper or paperboard to be tested, sufficient to provide one square for each of the required food-simulating solvents. (ii) Determination of color transfer. (a) Saturate the filter paper in the se lected solvent at room temperature (no lower than 65° F.) and place the saturated filter paper, "screen" side up, upon a piece of aluminum foil of appropriate size, handling the filter paper with tweezers.

(b) Using tweezers, promptly place the test square upon the wet filter paper being sure that the food-contact side of the test sample is in contact with the filter paper.

(c) Complete a four-ply "sandwich" by covering the upper side of the test paper with a cover of aluminum foil of suitable size.

(d) Seal the entire sandwich in complete cover of foil or in a polyethylene envelope to prevent loss of solvent during test period.

(e) Subject the sandwich to a pressure of 10 pounds per square inch of test paper and maintain the pressure continuously for at least 20 hours.

(f) At the conclusion of the contact period remove the pressure, carefully open the envelope, and remove the layers down to the filter paper by use of tweezers. (g) While still wet, compare the filter paper with the color transfer standard. If the color of the filter paper is not darker than the color transfer standard, the colorant shows no significant migration and meets the transfer test.

(4) Brightening-agent transfer. The test for brightening-agent transfer from treated paper and paperboard involves a visual comparison under ultraviolet light of a moist filter paper held in contact with the colored test paper for a period of time against a spot containing a known amount of fluorescent brightening agent.

(1) Equipment. (a) Glass-fiber filter paper.

(b) Aluminum foil.

(c) Tweezers.

(d) Appropriate solvents simulating the foods to be contacted by the paper or paperboard under test.

(e) Approximately 1-inch squares of the paper or paperboard to be tested, sufficient to provide one square for each of the required food-simulating solvents. (f) Fluorescent brightening-agent transfer standard: Prepare solution 1 as an aqueous solution of 10-50 milligrams per liter of Fluorescent Brightening Agent 28 and determine its absorbance in a 1-centimeter cell at a wavelength of 350 millimicrons in a suitable spectrophotometer against distilled water in the blank cell. Prepare a working solution by weighing out another amount of the brightening agent equal to :

11.8X concentration (grams per liter of
brightening agent in solution 1

Absorbance at 350 millimicrons

Transfer this amount to an actinic 500-milliliter volumetric flask. Make to volume and mix thoroughly as solution 2. Dilute 5 milliliters of solution 2 to 100 milliliters volumetrically with distilled water as soution 3. Dilute 10 milliliters of solution 3 to 100 milliliters with distilled water using an actinic flask for the preparation of solution 4 as the working-standard solution.

(ii) Determination of fluorescent brightening-agent transfer. (a) Using the "sandwich" technique described in subparagraph (3) of this paragraph, extract the brightening agent from the test paper onto the moist filter paper. (b) Place a drop of approximately 0.05 milliliter of the working standard solution (solution 4) on another glass-fiber filter paper and let dry. Moisten this spot with the same food-simulating solvent as used on the test paper and compare the standard spot with the moist filter paper under ultraviolet light. If the fluorescence of the test sample does not exceed the fluorescence of the standard spot, the fluorescent brightening agent shows no significant migration and meets the transfer test.

(5) Test for the discoloration of colorants. Prepare a solution (or suspension) containing approximately 10 milligrams colorant in 1 liter of the food-simulating solvent. Measure the absorbance of the solution at a suitable wavelength. Hold the solution at room temperature in the dark for 20 hours, then again measure absorbance at the predetermined wavelength. This test is repeated for each of the three food-simulating solvents (water, 1 percent citric acid solution, and lard oil), described in the footnotes to the table in subparagraph (1) of this paragraph. If with an solvent the absorbance after 20 hours dark storage is 10 percent or more below the original absorbance, the colorant may not be used in paper or paperboard intended for use in contact with food except for dry food of type VII identified in the table in subparagraph (1) of this paragraph.

All interested persons are invited to submit their views in writing, preferably in quintuplicate, regarding this proposal. Such views and comments should be addressed to the Hearing Clerk, Department of Health, Education, and Welfare, Room 5440, 330 Independence Avenue SW., Washington, D.C. 20201, within 30 days following the date of publication of this notice in the Federal Register. Comments may be accompanied by a memorandum or brief in support thereof. Dated: July 28, 1967. J. K. KIRK,

Associate Commissioner for Compliance.

[F.R. Doc. 67-9143; Filed, Aug. 3, 1967; 8:51 a.m.]

FDA GUIDELINES FOR CHEMISTRY AND TECHNOLOGY REQUIREMENTS OF FOOD ADDITIVE PETITIONS

The purpose of these guidelines is to elaborate and clarify the regulations with respect to the chemistry and technology requirements of food additive petitions. Section 121.51 of the Food Additive Regulations prescribes the required format, content, and organization of a food additive petition, in order to facilitate its scientific review and evaluation. The omission of any information required by the regulations must be adequately explained.

These guidelines are not to be construed as inflexible requirements, but they do reflect our views with respect to the type of data and other information needed for making an intelligent and informed evaluation of a food additive petition in the area of chemistry and technology. When a petitioner omits any of the data and information suggested by the guidelines or substitutes other types of data and information for those suggested by the guidelines, he should clearly explain the reasons for the omission or how such substituted data and information fufill the legal requirements of the regulations.

A general summary of the petition should be supplied by the petitioner. Among other things it should contain a statement with respect to the quantity of the food additive in individual foods or classes of foods under the proposed condi tions of use and the maximum as well as the average quantity to be expected in the total daily diet of the consumer; and a statement with respect to the margin of safety provided by the animal feeding studies. The clearance sought should be included and be specifically stated.

I. PROTOCOL FOR DIRECT ADDITIVES

A. Identity and composition

Information satisfying 121.51 in this area may be furnished in the form of a comprehensive monograph.

1. Name of the food additive:

(a) Common name: established or proposed, if any.

(b) Chemical name following the nomenclature of Chemical Abstracts. (c) Other names in use, including trade names.

2. Formula:

(a) Empirical formula.

(b) Structural formula, if known or proposed.

(c) Molecular weight.

3. Definition and description of the food additive, including its complete quantitative composition: liquid, solid, crystalline, amorphous, color, odor, taste, etc. Brief description of the manufacturing process, including a list of all substances used together with their specifications and the equations for all chemical reactions involved. Any production controls employed to assure a reproducible product should be described.

4. Physical, chemical, and/or biological properties, specifically including information or data on stability and also all other properties which may be appropriate, such as m.p., b.p., solubility, specific gravity, refractive index. viscosity, optical rotation, pH, acidity or alkalinity, ash, water content, iodine numbers, saponification number, alkoxyl content, volatile matter, water-soluble matter, ether-extractables, biological activity, absorption spectra in the ultra

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violet and infrared, flueorescence spectra, readily carbonizable substances, readily
oxidizable substances, etc. Will also appear in 5(a) or 5(c) when required.
5. Specifications for food grade:

(a) Identity. Include specifications useful in identifying the food additive and methods for checking the specifications.

(b) Assay. Specifications prescribing the minimum content of the desired component (s). Assay procedure described in full with validation data. Data showing the range of assays and that the assay specification can be met.

(c) Impurities. Specifications limiting total heavy metals (U.S.P. or ACS test) and specifically limiting arsenic and lead and also other undesirable impurities such as reaction byproducts to the lowest levels consistent with good manufacturing practice. Details of tests for checking the specifications. Data from a suitable number of representative batches showing the range of impurities and that the specifications can be met. 6. Any other pertinent information.

B. Usage and label specimen

Information should be furnished showing the quantity of the food additive proposed for use and the purpose for which it is proposed, together with all directions, recommendations, and suggestions regarding the proposed use, and a specimen of the proposed labeling. The maximum as well as the average quantity of the food additive to be expected in individual foods or types of foods and in the total daily diet of the consumer is to be estimated for the usage proposed; and the basis for the estimation is to be described in detail including any assumptions made and the arithmetical computations. Using adequate methodology, data should be submitted showing the fate of the food additive in finished food readyto-eat, whether the food additive remains unchanged in such food or whether it is converted to another substance by reason of oxidation, degradation, or reaction with components of the food, and the degree of any such conversion. C. Data on intended effect in food

Experimental data should be submitted showing that the food additive will produce the intended effect in food and that the usage level sought does not exceed the quantity of the additive reasonably required to produce such effect. Data from carefully controlled experiments showing the degree of effect accomplished by the additive at graduated levels of addition to food must be obtained. The number of graduated levels will depend upon a number of factors, such as the toxicity of the additive, the particular foods involved, the proposed usage level, and the increment of the additive required to induce any noticeable change in the effect on the foods. If the level of usage is considered by the petitioner to be self-limiting, the reasons should be explained and data furnished showing what excessive level of the additive will produce an unacceptable product.

Samples: To be furnished only on request. In order to assist us in evaluating the intended effect in food, we shall usually require samples of the food additive and samples of food reflecting usage of the additive, together with appropriate control samples.

The same samples may occasionally serve both the purpose of methodology testing discussed below and of demonstrating the intended technical effect in food.

D. Methodology

If usage of the food additive requires a tolerance for the food additive or for its conversion product(s) to protect the public health, a practicable method will have to be furnished to enforce the tolerance. It must be satisfactory for applica tion to the raw, processed, and/or finished food, i.e., give consistent results when used by any properly equipped and trained laboratory personnel. The method must be capable of quantitatively determining the food additive or its conversion product(s) in the presence of the normal components of the food in which it is to be used and in the presence of any other chemicals, including food additives, that can reasonably be expected to be present in such food. Validation data must be included, i.e., blanks (untreated food) and recoveries (food and additive at various levels, including level of usage), sufficient to demonstrate the accuracy and reproducibility of the method.

Appropriate samples may be requested for testing the method. (See C)