COMBINED COMPENDIUM OF FOOD ADDITIVE SPECIFICATIONS

Volume 4

COMBINED COMPENDIUM OF FOOD ADDITIVE SPECIFICATIONS

Joint FAO/WHO Expert Committee on Food Additives

All specifications monographs from the 1st to the 65th meeting (1956–2005)

Analytical methods, test procedures and laboratory solutions used by and referenced in the food additive specifications

FOOD AND AGRICULTURE ORGANIZATION OF THE UNITED NATIONS
Rome, 2006

Last updated (Web version): August 2011


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ISBN 92-5-105569-6

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FAO 2006

CONTENTS

ACKNOWLEDGEMENTS

SPECIAL NOTE

INTRODUCTION

GENERAL INFORMATION

Revision of Food and Nutrition Paper No. 5

Criteria for Replacement of Older Methods

Food Chemicals Codex

Hazardous Reagents and Solvents

Method Validation

ANALYTICAL TECHNIQUES

Chromatography

Introduction

Chromatography Principles

Chromatography Techniques

Column Chromatography

Paper Chromatography

Thin-Layer Chromatography

Gas Chromatography

Headspace-Gas Chromatography

Analysis of Samples – General Method Instructions

Gas Chromatography – Mass Spectrometry (GC-MS)

High Performance Liquid Chromatography

Spectrophotometry and Spectroscopy

Definitions

Terminology

Theory and Formulas for Calculation

Apparatus

UV/Visible Spectrophotometers

Atomic Absorption Spectrophotometers

Inductively Coupled Plasma – Atomic Emission Spectrophotometers

Spectrofluorimeters

Infrared Spectrometers

Nuclear Magnetic Resonance Spectrometers (NMR)

Procedures

Applications

GENERAL METHODS

Appearance and Physical Properties

Boiling Point and Distillation Range

Determination of pH (Potentiometric Method)

Melting Range/Melting Point

Refractive Index

Solidification Point

Solubility

Specific Gravity

Specific Rotation

Identification Tests

Inorganic Ions

Organic Ions and Compounds

Inorganic Components

Acid-Insoluble Matter

Arsenic Limit Test

Ash

Total Ash

Acid-insoluble Ash

Sulfated Ash

Chlorides Limit Test

Chromium Limit Test

Cyclic Phosphate Determination

Fluoride Limit Test

Method I – Thorium Nitrate Colorimetric Method

Method II – Ion-Selective Electrode Method, Method A

Method III – Ion-Selective Electrode Method, Method B

Method IV – Ion-Selective Electrode Method, Method C

Iron Limit Test

Loss on Drying

Loss on Ignition

Metallic Impurities

Measurement of Antimony, Barium, Cadmium, Chromium, Copper, Lead and Zinc by Atomic Absorption Flame Technique

Measurement of Antimony, Barium, Cadmium, Chromium, Copper, Lead and Zinc by Inductively Coupled Plasma Technique

Measurement of minerals and metals by Inductively Coupled Plasma –Atomic Emission spectrophotometric (ICP-AES) Technique

Measurement of Lead and Cadmium by Atomic Absorption Electro-Thermal (Furnace) Atomization Technique

Measurement of Arsenic and Antimony by Atomic Absorption Hydride Technique

Determination of Mercury by Cold Vapour Atomic Absorption Technique

Nickel in Polyols

Nickel Limit Test

Nitrogen Determination (Kjeldahl Method)

Method I

Method II (Semi-Micro)

Non-Volatile Residue

Phosphate Determination as P2O5

Method I

Method II

Phosphorous, calcium, magnesium and aluminium determination by Inductively Coupled Plasma-Atomic Emission Spectrophotometry (ICP-AES)

Selenium Limit Test

Sulfates Limit Test

Water-Insoluble Matter

Water Determination (Karl Fischer Titrimetric Method)

Organic Components

Chlorinated Organic Compounds Limit Test

Cyclohexylamine in Cyclamates

Dicyclohexylamine in Cyclamates

1,4-Dioxane and Ethylene Oxide

Fumaric and Maleic Acid

Gum Constituents Identification

Norbixin

Oxalate Limit Test

Polyols: Thin Layer Chromatography

Pyrrolidone Carboxylic Acid

Readily Carbonizable Substances

Reducing Substances (as Glucose)

Method I (Volumetric)

Method II (Gravimetric)

Related Foreign Substances in Flavour Enhancers

Residual Solvents

Method I (Determination carried out in water)

Method II (Determination carried out in methanol)

Toluenesulfonamides in Saccharines

Triphenylphosphine Oxide

Microbiological Analyses

Total (Aerobic) Plate Count

Spiral Plate Count Method (Alternative Method)

Coliforms and E-Coli

MPN Method (Alternative Method)

Salmonella

Staphylococcus aureus

Direct Plate Count Method

MPN Method

Enumeration of Yeasts and Moulds

SPECIFIC METHODS

Enzyme Preparations

α-Amylase Activity (Bacterial)

α-Amylase Activity (Fungal)

Antibacterial Activity

Catalase Activity

Cellulase Activity

Ethylenimine Limit Test

β-Galactocidase (Lactase) Activity

Glucoamylase Activity (Amyloglucosidase Activity)

β-Glucanase Activity

Glucose Isomerase Activity

Glucose Oxidase Activity

Gluteraldehyde Limit Test

Gluteraldehyde Determination in High Fructose Corn Syrup (High Fructose Glucose Syrup).

Hemicellulase Activity

Invertase Activity

Milk Clotting Activity

Protease Activity (Viscometer Method)

Proteolytic Activity, Bacterial (PC)

Proteolytic Activity, Fungal (HUT)

Proteolytic Activity, Fungal (SAP)

Proteolytic Activity, Plant

Pullulanase Activity

Xylanase Activity (Method 1)

Xylanase Activity (Method 2)

Fats, Oils and Hydrocarbons

Acid Value

Aromatic Hydrocarbons Determination

Average Molecular Weight

Carbon Number at 5% Distillation Point

Congealing Range

Free Fatty Acids

Hydroxyl Value

Identification Tests for Functional Groups

Test A – Methyl Esters of Fatty Acids

Test B – Acetic Acid

Test C – Succinic Acid

Test D – Fumaric Acid

Test E – Tartaric Acid

Test F – Citric Acid

Test G – Lactic Acid

Test H – Glycerol

Iodine Value (Modified Wijs Method)

1-Monoglyceride and Free Glycerol Contents

Polycyclic Aromatic Hydrocarbons

Polyglycerol Determination in Polyglycerol Esters

Polyols

Propylene Glycol Dimer and Trimer Determination

Saponification

Saponification Value

Sorbitan Ester Content

Sulfur

Viscosity, 100°

Flavouring Agents

Acid Value

Assay

Boiling Point

Ester Determination

Melting Point (Melting Range)

Refractive Index

Solubility in Ethano

Solubility in General

Specific Gravity

Food Colours

Chloride as Sodium Chloride

Chloroform-insoluble Matter

Colouring Matters

Identification by Chromatography

Identification by Spectrophotometry

Colouring Matters Content by Spectrophotometry

Colouring Matters Content of Water-soluble Colouring Matters

Colouring Matters Content of Organic Solvent-soluble Colouring Matters

Colouring Matters Content of Lakes

Colouring Matters Content by Titration with Titanous Chloride

Subsidiary Colouring Matter Content

Ether-extractable Matter

Hydrochloric acid-insoluble Matter in Lakes

Leuco Base in Sulfonated Triarylmethane Colours

Organic Compounds other than Colouring Matters

Sulfate as Sodium Sulfate

Unsulfonated Primary Aromatic Amines

Water Content (Loss on Drying)

Water-insoluble Matter

Water-soluble Chlorides and Sulfates in Aluminum Lakes

Glycerol Esters of Rosins

Ring and ball softening point method

ASSAY METHODS

Alginates Assay (Carbon Dioxide Determination by Decarboxylation)

Cellulose Derivatives Assay (Ethoxyl and Methoxyl Group Determination)

Polysorbates Assay (Oxyethylene Group Determination)

MEDIA, REAGENTS AND SOLUTIONS.

Media

Reagents

Buffer Solutions

Buffer Test Solutions

Standard Buffer Solutions

Standard Solutions

Test Solutions (TS)

Volumetric Solutions

Normal Solutions (N)

Molar Solutions (M)

Preparation and Methods of Standardization