Food Analysis Laboratory Manual

Second Edition

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Food Analysis Laboratory Manual

Second Edition

edited by

S. Suzanne Nielsen
Purdue University West Lafayette, IN, USA

S. Suzanne Nielsen Department of Food Science Purdue University West Lafayette IN USA

ISBN 978-1-4419-1462-0 e-ISBN 978-1-4419-1463-7 DOI 10.1007/978-1-4419-1463-7 Springer New York Dordrecht Heidelberg London
Library of Congress Control Number: 2009943246 Springer Science+Business Media, LLC 2010 All rights reserved. This work may not be translated or copied in whole or in part without the written permission of the publisher (Springer Science+Business Media, LLC, 233 Spring Street, New York, NY 10013, USA), except for brief excerpts in connection with reviews or scholarly analysis. Use in connection with any form of information storage and retrieval, electronic adaptation, computer software, or by similar or dissimilar methodology now known or hereafter developed is forbidden. The use in this publication of trade names, trademarks, service marks, and similar terms, even if they are not identified as such, is not to be taken as an expression of opinion as to whether or not they are subject to proprietary rights. Printed on acid-free paper Springer is part of Springer Science+Business Media (www.springer.com)

Contents
Preface and Acknowledgments vii Notes on Calculations of Concentration 1 8 ix Complexometric Determination of Calcium A B 9 EDTA Titrimetric Method for Testing Hardness of Water 63 Test Strips for Water Hardness 65 61 Nutrition Labeling Using a Computer Program 1 A B Preparing Nutrition Labels for Sample Yogurt Formulas 3 Adding New Ingredients to a Formula and Determining How They Influence the Nutrition Label 4 An Example of Reverse Engineering in Product Development 5 9 11

Iron Determination in Meat Using Ferrozine Assay 69

10

Sodium Determination Using Ion Selective Electrodes, Mohr Titration, and Test Strips 75 A B C Ion Selective Electrodes 77 Mohr Titration 79 Quantab Test Strips 81

Assessment of Accuracy and Precision

Determination of Moisture Content 17 A B C D E F G Forced Draft Oven 19 Vacuum Oven 21 Microwave Drying Oven 22 Rapid Moisture Analyzer 22 Toluene Distillation 22 Karl Fischer 23 Near Infrared Analyzer 25

Sodium and Potassium Determinations by Atomic Absorption Spectroscopy and Inductively Coupled Plasma-Atomic Emission Spectroscopy 87

12

Standard Solutions and Titratable Acidity 95 A B Preparation and Standardization of Base and Acid Solutions 97 Titratable Acidity and pH 99

Determination of Fat Content 29 A B C D Soxhlet Method 31 Goldfish Method 33 Mojonnier Method 34 Babcock Method 35

13

Fat Characterization 103 A B C D E Saponification Value 105 Iodine Value 106 Free Fatty Acid Value 108 Peroxide Value 109 Thin-Layer Chromatography Separation of Simple Lipids 111

Protein Nitrogen Determination 39 A B Kjeldahl Nitrogen Method 41 Nitrogen Combustion Method 43 14

Fish Muscle Proteins: Extraction, Quantitation, and Electrophoresis 115

Phenol-Sulfuric Acid Method for Total Carbohydrates 47

15

Enzyme Analysis to Determine Glucose Content 123

Vitamin C Determination by Indophenol Method 55

16

Gliadin Detection in Food by Immunoassay

129

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17 Examination of Foods for Extraneous Materials 137 A B C D E 18 Extraneous Matter in Soft Cheese 140 Extraneous Matter in Jam 140 Extraneous Matter in Infant Food 141 Extraneous Matter in Potato Chips 141 Extraneous Matter in Citrus Juice 142 145 20 Viscosity Measurement Using a Brookfield Viscometer 165 Calculation of CIE Color Specifications from Reflectance or Transmittance Spectra 19 Gas Chromatography A B 155

Contents

Determination of Methanol and Higher Alcohols In Wine by Gas Chromatography Preparation of Fatty Acid Methyl Esters (FAMEs), and Determination of Fatty Acid Profile of Oils by Gas Chromatography 159

157

High Performance Liquid Chromatography A B Determination of Caffeine in Beverages by HPLC 147 Solid-Phase Extraction and HPLC Analysis of Anthocyanidins from Fruits and Vegetables 149

21

171

Preface and Acknowledgments

This laboratory manual was written to accompany the textbook, Food Analysis, fourth edition. The laboratory exercises are tied closely to the text, and cover 20 of the 32 chapters in the textbook. Compared to the first edition of this laboratory manual, this second edition contains two new experiments, and previous experiments have been updated and corrected as appropriate. Most of the laboratory exercises include the following: background, reading assignment, objective, principle of method, chemicals (with CAS number and hazards), reagents, precautions and waste disposal, supplies, equipment, procedure, data and calculations, questions, and resource materials. Instructors using these laboratory exercises should note the following: 1. It is recognized that the time and equipment available for teaching food analysis laboratory sessions vary considerably between schools, as do the student numbers and their level in school. Therefore, instructors may need to modify the laboratory procedures (e.g., number of samples analyzed; replicates) to fit their needs and situation. Some experiments include numerous parts/methods, and it is not assumed that an instructor uses all parts of the experiment as written. It may be logical to have students work in pairs to make things go faster. Also, it may be logical to have some students do one part of the experiment/one type of sample, and other students to another part of the experiment/type of sample. 2. The information on hazards and precautions in use of the chemicals for each experiment is not comprehensive, but should make students and a laboratory assistant aware of major concerns in handling and disposal of the chemicals. 3. It is recommended in the text of the experiments that a laboratory assistant prepare many of the reagents, because of the time limitations for students in a laboratory session. The lists of supplies and equipment for experiments do not necessarily include those needed by the laboratory assistant in preparing reagents, etc. for the laboratory session. 4. The data and calculations section of the laboratory exercises provides details on recording data and doing calculations. In requesting laboratory reports from students, instructors will need to specify if they require just sample calculations or all calculations. 5. Students should be referred to the definitions on percent solutions and on converting parts per million solutions to other units of concentration as given in the notes that follow the preface. Even though this is the second edition of this laboratory manual, there are sure to be inadvertent omissions and mistakes. I will very much appreciate receiving suggestions for revisions from instructors, including input from lab assistants and students. I am grateful to the food analysis instructors identified in the text who provided complete laboratory experiments or the materials to develop the experiments. The input I received from Dr. Charles Carpenter of Utah State University for the first edition of this laboratory manual about the content of the experiments continued to be helpful for this second edition. Likewise, my former graduate students are thanked again for their help in working out and testing the experimental procedures written for the first edition. For this second edition, I want to especially thank my graduate student, Cynthia Machado, for her assistance and offering advice based on her experience in serving as a teaching assistant for a Food Analysis laboratory course. West Lafayette, IN S. Suzanne Nielsen

vii

Notes on Calculations of Concentration

Definitions of Percent Solutions: Weight/Volume Percent (%, w/v) = weight, in g of a solute, per 100 ml of solution Weight/Weight Percent (%, w/w) = weight, in g of a solute, per 100 g of solution Volume/Volume Percent (%, v/v) = volume, in ml of a solute, per 100 ml of solution Concentration of minerals is expressed commonly as parts per billion (ppb) or parts per million (ppm). Parts per million is related to other units of measure as follows: = 1000 ppm = ppm = g mg mg = = g 1000 g L 1000 g 1 mg 0.001 g = = g g g 0.1 g = 0.1% 100 g

ix