Food Chemicals Codex Methods

VALIDATION OF FOOD CHEMICALS CODEX METHODS Submissions to the Food Chemicals Codex... 

Analytical Procedures. Standard methods for analysis of food-grade adipic acid are described ia the Food Chemicals Codex (see Refs, ia Table 8). Classical methods are used for assay (titration), trace metals (As, heavy metals as Pb), and total ash. Water is determined by Kad-Fisher titration of a methanol solution of the acid. Determination of color ia methanol solution (APHA, Hazen equivalent, max. 10), as well as iron and other metals, are also described elsewhere (175). Other analyses frequendy are required for resia-grade acid. For example, hydrolyzable nitrogen (NH, amides, nitriles, etc) is determined by distillation of ammonia from an alkaline solution. Reducible nitrogen (nitrates and nitroorganics) may then be determined by adding DeVarda s alloy and continuing the distillation. Hydrocarbon oil contaminants may be determined by ir analysis of halocarbon extracts of alkaline solutions of the acid. 

Specifications for sulfuric acid vary rather widely. Exceptions include the federal specifications for "Sulfuric Acid, Technical" and "Sulfuric Acid, Electrolyte (for storage batteries)" and the Food Chemicals Codex specification for sulfuric acid, frequentiy called food-grade acid (although industrywide, "food-grade" is nonspecific). Very Httie has been done to estabUsh industry-wide analytical standards in the United States, except for development of the ASTM analytical methods, designated as E223-88 and summarized in Table 12. 

Nutrients and diet supplements without claims of therapeutic effects are considered foods, and are thus regulated by the U.S. Food and Dmg Administration. These are further subject to specific food regulations. Specifications for pyridoxine hydrochloride (7) for foods are given in the Food Chemicals Codex (80) and for pharmaceuticals in the US. Pharmacopeia (81). General test methods have been summarized (82). 

The United States Pharmacopeia XXIII (USP XXIII-NF XVHI), The United States Pharmacopeia Convention, Inc., Rockville, Md., 1995, p. 1631. Pood and Nutrition Board, National Research Council, Food Chemicals Codex, 3rd ed.. National Academy Press, Washiagton, D.C., 1981, p. 330. K. Helrich, ed.. Official Methods of Analysis of the Association of Off dal Analytical Chemists, 15th ed.. Association of Official Analytical Chemists, Inc., Arlington, Va., 1990, pp. 1070—1079. 

Food and pharmaceutical grades of calcium carbonate are covered by the Food Chemicals Codex (7) and the United States Pharmacopeia (8) and subject to U.S. Food and Dmg Administration Good Manufacturing Practices (9). Both purity requirements and test methods are available (7,8). Calcium carbonate is listed in the U.S. Code of Federal Regulation as a food additive, and is authorized for use in both paper and plastic food contact appHcations. 

Specifications and Standards Test Methods. Ethylcellulose is cleared foi many apphcations in food and food contact under the Eedeial Eood, Dmg, and Cosmetic Act, as amended. Examples include binder in dry vitamin preparations for animal feed, coatings and inks for paper and paperboard products used in food packaging, and closures with sealing gaskets for food containers (44). Methods of analyses ate given in ASTM D914-72 (19), NationalFonmila XIV, and Food Chemicals Codex II. 

Specifications and Standards Test Methods. Pood-grade HPC products are manufactured for use in food and conform to the specifications for HPC set forth in CPR 21, Section 172.870. Pood grades of HPC also conform to the specifications for HPC as Usted in the current edition of the Food Chemicals Codex. 

Analytical methods. The anhydrouronic acid content (AUAC), degree of esterification (DE), degree of amidation (DA) and ash content were determined according to the methods described in Food Chemical Codex II ed [5]. 

While the above EU Directive lists the criteria only, the JECFA specifications refer to analytical methods in a Guide to Specifications35 or describe the analytical method in the specification monograph itself. Similarly, the Food Chemicals Codex lists and describes the necessary analytical methods for purity control. 

Benzaldehyde is sold as technical grade or as meeting the specifications of the NationalFormulary (NF) (7), the Food Chemicals Codex (FCC) (8), or the British Pharmacopeia (BP) (9) (Tables 4 and 5). The test methods used for the analysis of benzaldehyde are standard methods, with the exception of the assay method. 

Iodine Value (or Number)—the percentage of iodine that will be absorbed by a clieimcally unsalurated substance, such as vegetable oil, in a given time under specified conditions. The iodine value is a measure of degree of unsaturation. Two methods are described in the Food Chemicals Codex the Hanus method and the Wijs method. 

In addition to chemical assays, Basic Protocols 4 through 6 evaluate the physical properties of citms oils. These methods are based on the high percentage of rf-limonene, in which citms oils have characteristic values. Table Gl.5.7 provides the physical and chemical properties defined by Food Chemical Codex (NRC, 1981). 

The specific gravity of steam-distilled oil was a little higher than that of the oil from liquid C02 extraction. The specific gravities of the samples from the two methods were similar to the standard values of anise essential oil reported by the FCC (Food Chemicals Codex), as cited by Heath (1981). The refractive indices, as well as the optical rotation of the oils from steam distillation and those from liquid C02 were not significantly different. All values of optical rotation were of levo orientation. 

Although the assays and tests described constitute methods upon which the specifications of the Food Chemicals Codex depend, analysts are not prevented from applying alternative methods if they are satisfied that the procedures used will produce results of equal or greater accuracy. In the event of doubt or disagreement concerning a substance purported to comply with the requirements of this Codex, only the methods described herein are applicable and authoritative. 

Allergens The Committee on Food Chemicals Codex recognizes the issue of food allergens, but current limitations regarding (1) the threshold levels and (2) the analytical methods to detect allergens at very low levels have thus far prevented the inclusion in FCC monographs of specifications related to allergens. 

Reagents Specifications for reagents are not included in the Food Chemicals Codex. Unless otherwise specified, reagents required in tests and assays should conform to the specifications of the current editions of Reagent Chemicals—American Chemical Society Specifications or in the section on Reagent Specifications in the United States Pharmacopeia. Reagents not covered by any of these specifications should be of a grade suitable to the proper performance of the method of assay or test involved. 

It obviously is impossible to provide limits and tests in each monograph for the detection of all possible unusual or unexpected impurities, the presence of which would be inconsistent with good manufacturing practice. The limits and tests provided are those considered to be necessary according to currently recognized methods of manufacture and are based on information available to or provided to the Committee on Food Chemicals Codex. If other methods of manufacture or other than the usual raw materials are used, or if other possible impurities may be present, additional tests may be required and should be applied, as necessary, by the manufacturer, vendor, or user to demonstrate that the substance is suitable for its intended application. 

The Committee on Food Chemicals Codex notes that this method may be used only until the First Supplement to this edition is released in 2004. At that time, the committee will set a lead limit as low as practicable for potassium chloride. Manufacturers are encouraged to develop and validate methods for use in industrial settings and that are sensitive enough to detect lead in the amounts typically present in potassium chloride, and to propose such methods to the committee in a timely manner. 

Thermometers suitable for Food Chemicals Codex use conform to the specifications of the American Society for Testing and Materials, ASTM Standards E 1, and are standardized in accordance with ASTM Method E 77. 

HI. The level of HI matter is one measure of the purity of lecithin products. HI matter usually consists of residual fiber, but also particulate contaminants that may be introduced during processing (e.g., filter aids). The level of HI matter in crude lecithin should never exceed 0.3% and rarely exceeds 0.1%. HI matter in lecithin is detrimental to clarity and use in specific applications. HI is measured by an official Food Chemicals Codex (FCC) (1996) method (54) or by AOCS Official Method Ja 3-87 (77). 

There are a variety of analytical methods commonly used for the characterization of neat soap and bar soaps. Many of these methods have been published as official methods by the American Oil Chemists Society (23). Additionally, many analysts choose United States Pharmacopoeia (USP), British Pharmacopoeia (BP), or Food Chemical Codex (FCC) methods. These methods tend to be colorimetric, potentio-metric, or titrametric procedures. However, a variety of instrumental techniques are also frequently used, e.g., gas chromatography, high-performance liquid chromatography, nuclear magnetic resonance spectroscopy, infrared spectroscopy, and mass spectrometry. 

The physical analysis of the seeds was conducted by measuring the diameters of 10-15 seeds from each sample at the widest point and weighing each seed. Seed coat and endosperm color were visually evaluated. The moisture, total ashes, and total insoluble ashes were assessed using methods described by the Food Chemical Codex (P). 

FCC. (1) Abbreviation for Food Chemicals Codex, a publication giving specifications and test methods for chemicals used in foods. (2) Abbreviation for fluid-cracking catalyst as used in the petroleum refining industry. Examples are powdered silica alumina, in which alumina is impregnated with dry synthetic silica gel, and various natural clays impregnated with alumina. 

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