Food Analysis Laboratory Manual

242 Pages·2017·8.85 MB·English

by  S. Suzanne Nielsen (auth.)

Food Science Text Series
S. Suzanne Nielsen
Food Analysis
Laboratory Manual
Third Edition
Food Science
Text Series
Third Edition
For other titles published in this series, go to
www.springer.com/series/5999
Series editor:
Dennis  R. Heldman
Heldman Associates
Mason, Ohio, USA
The Food Science Text Series provides faculty with the leading teaching tools. The Editorial Board has
outlined the most appropriate and complete content for each food science course in a typical food science
program and has identified textbooks of the highest quality, written by the leading food science educators.
Series Editor Dennis R. Heldman, Professor, Department of Food, Agricultural, and Biological Engineering,
The Ohio State University. Editorial Board; John Coupland, Professor of Food Science, Department of Food
Science, Penn State University, David A. Golden, Ph.D., Professor of Food Microbiology, Department of Food
Science and Technology, University of Tennessee, Mario Ferruzzi, Professor, Food, Bioprocessing and
Nutrition Sciences, North Carolina State University, Richard W. Hartel, Professor of Food Engineering,
Department of Food Science, University of Wisconsin, Joseph H. Hotchkiss, Professor and Director of the
School of Packaging and Center for Packaging Innovation and Sustainability, Michigan State University,
S. Suzanne Nielsen, Professor, Department of Food Science, Purdue University, Juan L. Silva, Professor,
Department of Food Science, Nutrition and Health Promotion, Mississippi State University, Martin
Wiedmann, Professor, Department of Food Science, Cornell University, Kit Keith L. Yam, Professor of Food
Science, Department of Food Science, Rutgers University
Food Analysis
Laboratory Manual
Third Edition
edited by
S. Suzanne Nielsen
Purdue University
West Lafayette, IN, USA
S. Suzanne Nielsen
Department of Food Science
Purdue University
West Lafayette
Indiana
USA
ISSN 1572-0330 ISSN 2214-7799 (electronic)
Food Science Text Series
ISBN 978-3-319-44125-2 ISBN 978-3-319-44127-6 (eBook)
DOI 10.1007/978-3-319-44127-6
Library of Congress Control Number: 2017942968
© Springer International Publishing 2017
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Preface and Acknowledgments
This laboratory manual was written to accompany able for teaching food analysis laboratory
the textbook, Food Analysis, fifth edition. The labora- sessions vary considerably between schools,
tory exercises are tied closely to the text and cover 21 as do student numbers and their level in
of the 35 chapters in the textbook. Compared to the school. Therefore, instructors may need to
second edition of this laboratory manual, this third modify the laboratory procedures (e.g., num-
edition contains four introductory chapters with ber of samples analyzed, replicates) to fit their
basic information that compliments both the text- needs and situation. Some experiments
book chapters and the laboratory exercises (as include numerous parts/methods, and it is
described below). Three of the introductory chapters not assumed that an instructor uses all parts
include example problems and their solutions, plus of the experiment as written. It may be logical
additional practice problems at the end of the chap- to have students work in pairs to make things
ter (with answers at the end of the laboratory man- go faster. Also, it may be logical to have some
ual). This third edition also contains three new students do one part of the experiment/one
laboratory exercises, and previous experiments have type of sample and other students to another
been updated and corrected as appropriate. Most of part of the experiment/type of sample.
the laboratory exercises include the following: back- 4. Use of Chemicals: The information on hazards
ground, reading assignment, objective, principle of and precautions in the use of the chemicals for
method, chemicals (with CAS number and hazards), each experiment is not comprehensive but
reagents, precautions and waste disposal, supplies, should make students and a laboratory assis-
equipment, procedure, data and calculations, ques- tant aware of major concerns in handling and
tions, and resource materials. disposing of the chemicals.
Instructors using these laboratory exercises 5. Reagent Preparation: It is recommended in the
should note the following: text of the experiments that a laboratory assis-
tant prepare many of the reagents, because of
1. Use of Introductory Chapters: the time limitations for students in a laboratory
• Chap. 1, “Laboratory Standard Operating session. The lists of supplies and equipment for
Procedures” – recommended for students experiments do not necessarily include those
prior to starting any food analysis labora- needed by the laboratory assistant in preparing
tory exercises reagents for the laboratory session.
• Chap. 2, “Preparation of Reagents and 6. Data and Calculations: The laboratory exer-
Buffers” – includes definition of units of cises provide details on recording data and
concentrations, to assist in making chemi- doing calculations. In requesting laboratory
cal solutions reports from students, instructors will need to
• Chap. 3, “Dilution and Concentration specify if they require just sample calculations
Calculations” – relevant for calculations in or all calculations.
many laboratory exercises
• Chap. 4, “Use of Statistics in Food Even though this is the third edition of this labo-
Analysis” – relevant to data analysis ratory manual, there are sure to be inadvertent omis-
2. Order of Laboratory Exercises: The order of sions and mistakes. I will very much appreciate
laboratory exercises has been changed to be receiving suggestions for revisions from instructors,
fairly consistent with the reordering of chap- including input from lab assistants and students.
ters in the textbook, Food Analysis, fifth edition I maintain a website with additional teaching
(i.e., chromatography and spectroscopy near materials related to both the Food Analysis textbook
the front of the book). However, each labora- and laboratory manual. Instructors are welcome to
tory exercise stands alone, so they can be cov- contact me for access to this website. To compliment
ered in any order. the laboratory manual, the website contains more
3. Customizing Laboratory Procedures: It is rec- detailed versions of select introductory chapters and
ognized that the time and equipment avail- Excel sheets related to numerous laboratory exercises.
v
vi Preface and Acknowledgments
I am grateful to the food analysis instructors much appreciated. Special thanks go to Baraem
identified in the text who provided complete labora- (Pam) Ismail and Andrew Neilson for their input
tory experiments or the materials to develop the and major contributions toward this edition of the
experiments. For this edition, I especially want to laboratory manual. My last acknowledgment goes to
thank the authors of the new introductory chapters my former graduate students, with thanks for their
who used their experience from teaching food analy- help in working out and testing all experimental pro-
sis to develop what I hope will be very valuable cedures written for the initial edition of the labora-
chapters for students and instructors alike. The input tory manual.
I received from other food analysis instructors, their
students, and mine who reviewed these new intro- West Lafayette, IN, USA S. Suzanne Nielsen
ductory chapters was extremely valuable and very
Contents
Preface and Acknowledgments v 4.6 t -Scores 58
4.7 t -Tests 59
4.8 P ractical Considerations 61
Part 1 Introductory Chapters
4.9 P ractice Problems 62
4.10 Terms and Symbols 62
1 Laboratory Standard Operating Procedures 3
1.1 I ntroduction 5
1.2 P recision and Accuracy 5 Part 2 Laboratory Exercises
1.3 B alances 6
1.4 M echanical Pipettes 7 5 Nutrition Labeling Using a Computer
1.5 G lassware 9 Program 65
1.6 R eagents 16 5.1 Introduction 67
1.7 D ata Handling and Reporting 18 5.2 Preparing Nutrition Labels for Sample
1.8 B asic Laboratory Safety 19 Yogurt Formulas 67
5.3 Adding New Ingredients to a Formula
and Determining How They Influence
2 Preparation of Reagents and Buffers 21
the Nutrition Label 68
2.1 Preparation of Reagents of Specified
5.4 An Example of Reverse Engineering
Concentrations 22
in Product Development 69
2.2 U se of Titration to Determine
5.5 Questions 70
Concentration of Analytes 24
2.3 P reparation of Buffers 25
2.4 N otes on Buffers 30 6 A ccuracy and Precision Assessment 71
2.5 P ractice Problems 31 6.1 I ntroduction 72
6.2 P rocedure 73
6.3 D ata and Calculations 74
3 D ilutions and Concentrations 33
6.4 Questions 74
3.1 I ntroduction 34
3.2 R easons for Dilutions
and Concentrations 34 7 H igh-Performance Liquid
3.3 U sing Volumetric Glassware Chromatography 77
to Perform Dilutions 7.1 Introduction 79
and Concentrations 34 7.2 Determination of Caffeine in Beverages
3.4 C alculations for Dilutions By HPLC 79
and Concentrations 34 7.3 Solid-Phase Extraction and HPLC Analysis
3.5 S pecial Cases 40 of Anthocyanidins from Fruits
3.6 S tandard Curves 41 and Vegetables 81
3.7 U nit Conversions 44
3.8 A voiding Common Errors 45
8 G as Chromatography 87
3.9 P ractice Problems 46
8.1 Introduction 89
8.2 Determination of Methanol and Higher
4 Statistics for Food Analysis 49 Alcohols in Wine by Gas
4.1 I ntroduction 50 Chromatography 89
4.2 P opulation Distributions 50 8.3 Preparation of Fatty Acid Methyl
4.3 Z -Scores 51 Esters (FAMEs) and Determination
4.4 S ample Distributions 54 of Fatty Acid Profile of Oils by Gas
4.5 C onfidence Intervals 55 Chromatography 91
vii
viii Contents
9 Mass Spectrometry with High-Performance 16 Water Hardness Testing by Complexometric
Liquid Chromatography 97 Determination of Calcium 147
9.1 I ntroduction 98 16.1 Introduction 149
9.2 P rocedure 100 16.2 EDTA Titrimetric Method for Testing
9.3 D ata and Calculations 101 Hardness of Water 149
9.4 Q uestions 102 16.3 Test Strips for Water Hardness 151
9.5 C ase Study 102
17 Phosphorus Determination by Murphy-Riley
10 Moisture Content Determination 105 Method 153
10.1 I ntroduction 107 17.1 Introduction 154
10.2 F orced Draft Oven 107 17.2 Procedure 155
10.3 V acuum Oven 109 17.3 Data and Calculations 155
10.4 M icrowave Drying Oven 110 17.4 Questions 155
10.5 R apid Moisture Analyzer 111
10.6 T oluene Distillation 111
18 Iron Determination by Ferrozine Method 157
10.7 K arl Fischer Method 112
18.1 Introduction 158
10.8 N ear-Infrared Analyzer 114
18.2 Procedure 158
10.9 Q uestions 114
18.3 Data and Calculations 159
18.4 Question 159
11 Ash Content Determination 117
11.1 I ntroduction 118
19 Sodium Determination Using Ion-Selective
11.2 Procedure 118
Electrodes, Mohr Titration, and Test Strips 161
11.3 Data and Calculations 118
19.1 Introduction 163
11.4 Questions 119
19.2 Ion-Selective Electrodes 163
19.3 Mohr Titration 165
12 Fat Content Determination 121 19.4 Quantab® Test Strips 167
12.1 I ntroduction 123 19.5 Summary of Results 169
12.2 S oxhlet Method 123 19.6 Q uestions 170
12.3 G oldfish Method 125
12.4 Mojonnier Method 125
20 Sodium and Potassium Determinations
12.5 B abcock Method 127
by Atomic Absorption Spectroscopy
and Inductively Coupled Plasma- Optical
13 Protein Nitrogen Determination 131 Emission Spectroscopy 171
13.1 I ntroduction 132 20.1 Introduction 173
13.2 Kjeldahl Nitrogen Method 132 20.2 Procedure 174
13.3 N itrogen Combustion Method 135 20.3 Data and Calculations 176
20.4 Questions 177
14 Total Carbohydrate by Phenol-Sulfuric
Acid Method 137 21 Standard Solutions and Titratable Acidity 179
14.1 Introduction 138 21.1 Introduction 180
14.2 Procedure 139 21.2 Preparation and Standardization of Base
14.3 Data and Calculations 140 and Acid Solutions 180
14.4 Questions 141 21.3 T itratable Acidity and pH 182
15 V itamin C Determination by Indophenol 22 F at Characterization 185
Method 143 22.1 I ntroduction 187
15.1 I ntroduction 144 22.2 S aponification Value 187
15.2 P rocedure 145 22.3 Iodine Value 188
15.3 D ata and Calculations 145 22.4 Free Fatty Acid Value 190
15.4 Q uestions 146 22.5 Peroxide Value 191
22.6 Thin-Layer Chromatography Separation
of Simple Lipids 193
Contents ix
23 Proteins: Extraction, Quantitation, 27 CIE Color Specifications Calculated
and Electrophoresis 195 from Reflectance or Transmittance Spectra 219
23.1 Introduction 196 27.1 I ntroduction 221
23.2 Reagents 197 27.2 P rocedure 222
23.3 Supplies 198 27.3 Q uestions 224
23.4 P rocedure 198
23.5 Data and Calculations 200
28 Extraneous Matter Examination 225
23.6 Q uestions 200
28.1 Introduction 227
28.2 Extraneous Matter in Soft Cheese 227
24 Glucose Determination by Enzyme 28.3 Extraneous Matter in Jam 228
Analysis 203 28.4 Extraneous Matter in Infant Food 229
24.1 I ntroduction 204 28.5 Extraneous Matter in Potato Chips 229
24.2 P rocedure 205 28.6 Extraneous Matter in Citrus Juice 230
24.3 D ata and Calculations 205 28.7 Questions 230
24.4 Q uestions 205
Part 3 Answers to Practice Problems
25 Gliadin Detection by Immunoassay 207
29 Answers to Practice Problems in Chap. 2,
25.1 Introduction 208
Preparation of Reagents and Buffers 233
25.2 Procedure 209
25.3 Data and Calculations 210
25.4 Questions 211 30 Answers to Practice Problems in Chap. 3,
Dilutions and Concentrations 239
26 Viscosity Measurements of Fluid Food
Products 213 31 Answers to Practice Problems in Chap. 4,
26.1 I ntroduction 214 Use of Statistics in Food Analysis 247
26.2 P rocedure 214
26.3 D ata 216
26.4 C alculations 216
26.5 Q uestions 217