Food Analysis

Food Science Text Series

S. Suzanne Nielsen

Editor

Fifth Edition

Food Analysis

Food Science

Text Series

Fifth 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, Professor of Food Microbiology, Department of Food

Science and Technology, University of Tennessee. Mario Ferruzzi, Professor, Food Bioprocessing and

Nutritional 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

Fifth Edition

Edited by

S. Suzanne Nielsen

Purdue University

West Lafayette, IN, USA

Editor

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 978-3-319-45774-1 ISBN 978-3-319-45776-5 (eBook)

DOI 10.1007/978-3-319-45776-5

Library of Congress Control Number: 2017942967

© Springer International Publishing 2017, corrected publication 2019

This work is subject to copyright. All rights are reserved by the Publisher, whether the whole or part of the material is concerned,

specifically the rights of translation, reprinting, reuse of illustrations, recitation, broadcasting, reproduction on microfilms or in any other

physical way, and transmission or information storage and retrieval, electronic adaptation, computer software, or by similar or dissimilar

methodology now known or hereafter developed.

The use of general descriptive names, registered names, trademarks, service marks, etc. in this publication does not imply, even in the

absence of a specific statement, that such names are exempt from the relevant protective laws and regulations and therefore free for

general use.

The publisher, the authors and the editors are safe to assume that the advice and information in this book are believed to be true and

accurate at the date of publication. Neither the publisher nor the authors or the editors give a warranty, express or implied, with respect

to the material contained herein or for any errors or omissions that may have been made. The publisher remains neutral with regard to

jurisdictional claims in published maps and institutional affiliations.

Printed on acid-free paper

This Springer imprint is published by Springer Nature

The registered company is Springer International Publishing AG

The registered company address is: Gewerbestrasse 11, 6330 Cham, Switzerland

v

The intent of this fifth edition book is the same as

that described in the Preface to the first four edi￾tions – a text primarily for undergraduate students

majoring in food science, currently studying the

analysis of foods. However, comments from users

of the first four editions have convinced me that the

book is also a valuable text for persons in the food

industry who either do food analysis or interact

with analysts.

The big focus of this edition was to do a gen￾eral update on methods and to make the content

easier for readers to compare and contrast methods

covered. The following summarize changes from

the fourth edition: (1) general updates, including

addition and deletion of methods, (2) three new

chapters (“Determination of Total Phenolics and

Antioxidants Capacity in Food and Ingredients,”

“Food Microstructure Techniques,” “Food Forensic

Investigation”), (3) rewrote and/or reorganized

some chapters, (4) added tables to some chapters to

summarize and compare methods, and (5) added

some colored figures.

As stated for the first four editions, the chap￾ters in this textbook are not intended as detailed

references, but as general introductions to the

topics and the techniques. Course instructors

may wish to provide more details on a particular

topic to students. Chapters focus on principles

and applications of techniques. Procedures given

are meant to help explain the principles and give

some examples, but are not meant to be presented

in the detail adequate to actually conduct a specific

analysis. As in the first four editions, all chapters

have summaries and study questions, and key￾words or phrases are in bold type, to help students

focus their studies. The grouping of chapters by

category is similar to the fourth edition. However,

due to the increased use of spectroscopy and

chromatography for many basic analyses, chap￾ters on these topics are covered early in the book.

Instructors are encouraged to cover the topics from

this text in whatever order is most suitable for their

course. Also, instructors are invited to contact me

for access to a website I maintain with additional

teaching materials related to this textbook and the

accompanying laboratory manual.

Starting with the third edition, the competency

requirements established by the Institute of Food

Technologists were considered. Those requirements

relevant to food analysis are as follows: (1) under￾standing the principles behind analytical techniques

associated with food, (2) being able to select the

appropriate analytical technique when presented

with a practical problem, and (3) demonstrating

practical proficiency in food analysis laboratory. This

textbook should enable instructors to meet the

requirements and develop learning objectives rele￾vant to the first two of these requirements. The labo￾ratory manual, now in its third edition, should be a

useful resource to help students meet the third

requirement.

I am grateful to all chapter authors for agree￾ing to be a part of this project. Authors have

drawn on their experience of teaching students

and/or experience with these analyses to give

chapters the appropriate content, relevance, and

ease of use. I wish to thank the authors of articles

and books, as well as the publishers and indus￾trial companies, for their permission to reproduce

materials used here. Special thanks is extended to

the following persons: Baraem (Pam) Ismail for

valuable discussions about the content of the

book and reviewing several book chapters, Ben

Paxson for drawing/redrawing figures, and

Telaina Minnicus and Mikaela Allan for word

processing assistance. I am also very grateful to

Bill Aimutis, Angela Cardinali, Wayne Ellefson,

Chris Fosse, and David Plank who were valuable

for discussions and arranged for me to visit with

numerous scientists in the analytical laboratories

at the following companies/institute: Cargill,

ConAgra Foods, Covance, and General Mills in

the USA, and Bonassisa Lab and the Institute of

Science of Food Production in Italy.

West Lafayette, IN, USA S. Suzanne Nielsen

Preface and Acknowledgments

vi

The original version of this book was revised.

The correction to this book can be found at DOI https://doi.org/10.1007/978-3-319-45776-5_36

Preface and Acknowledgments

vii

2-D Two-dimensional

3-D Three-dimensional

3-MCPD 3-Monochloropropane 1,2-diol

AACC American Association of Cereal

Chemists

AACCI AACI International

AAS Atomic absorption spectroscopy

AAPH 2,2′-Azobis (2-amidinopropane)

dihydrochloride

ABTS 2,2′-Azino-bis (3-ethylbenzenothazoline￾6-sulfonic acid)

ADI Acceptable daily intake

ADP Adenosine-5′-diphosphate

AE-HPLC Anion exchange high-performance liq￾uid chromatography

AES Atomic emission spectroscopy

AFM Atomic force microscopy

AMS Accelerator mass spectrometer

AMS Agricultural Marketing Service

AOAC Association of Official Analytical

Chemists

AOCS American Oil Chemists’ Society

AOM Active oxygen method

APCI Atmospheric pressure chemical

ionization

APHA American Public Health Association

API Atmospheric pressure ionization

APPI Atmospheric pressure photoionization

AQC 6-Aminoquinolyl-N-hydroxysuccin￾imidyl carbamate

ASE Accelerated solvent extraction

ASTM American Society for Testing Materials

ATCC American Type Culture Collection

ATP Adenosine-5′-triphosphate

ATR Attenuated total reflectance

AUC Area under the curve

aw Water activity

B0 External magnetic field

BAW Base and acid washed

BCA Bicinchoninic acid

BCR Community Bureau of Reference

Bé Baumé modulus

BHA Butylated hydroxyanisole

BHT Butylated hydroxytoluene

BOD Biochemical oxygen demand

BPA Bisphenol A

BSA Bovine serum albumin

BSDA Bacillus stearothermophilus disk assay

BSE Backscattered electrons

BSTFA N,O-Bis(trimethylsilyl)

trifluoroacetamide

CAD Collision-activated dissociation

CAST Calf antibiotic and sulfa test

CAT Computerized axial tomography

CCD Charge-coupled device

CDC Centers for Disease Control

CFR Code of Federal Regulations

CFSAN Center for Food Safety and Applied

Nutrition

cGMP Current Good Manufacturing Practices

CI Confidence interval

CI Chemical ionization

CID Collision-induced dissociation

CID Commercial item description

CID Charge injection device

CIE Commission Internationale d’Eclairage

CLA Conjugated linoleic acid

CLND Chemiluminescent nitrogen detector

CLSM Confocal laser scanning microscopy

CMC Critical micelle concentration

COA Certificate of analysis

COD Chemical oxygen demand

C-PER Protein efficiency ratio calculation

method

CPG Compliance policy guidance

CP-MAS Cross-polarization magic angle spinning

CQC 2,6-Dichloroquinonechloroimide

CRC Collision reaction cells

CSLM Confocal scanning laser microscopy

CT Computed technology

CT Computed tomography

CV Coefficient of variation

CVM Center for Veterinary Medicine

DAL Defect action level

DART Direct analysis in real time

DDT Dichlorodiphenyltrichloroethane

DE Degree of esterification

dE* Total color difference

DF Dilution factor

DFE Dietary folate equivalent

DHHS Department of Health and Human

Services

DIAAS Digestible indispensable amino acid score

DIC Differential interferential contrast

Abbreviations

DMA Dynamic mechanical analysis

DMF Dimethylformamide

DMD D-Malate dehydrogenase

DMSO Dimethyl sulfoxide

DNA Deoxyribonucleic acid

DNFB 1-Fluoro-2,4-dinitrobenzene

dNTPs Deoxynucleoside triphosphates

DON Deoxynivalenol

DRI Dietary references intake

DRIFTS Diffuse reflectance infrared Fourier

transform spectroscopy

DRV Daily reference value

DSC Differential scanning calorimetry

DSHEA Dietary Supplement Health and

Education Act

DSPE Dispersive solid-phase extraction

DTGS Deuterated triglycine sulfate

DV Daily value

DVB Divinylbenzene

DVS Dynamic vapor sorption

dwb Dry weight basis

Ea Activation energy

EAAI Essential amino acid index

EBT Eriochrome black T

ECD Electron capture dissociation

ECD Electron capture detector

ECD (Pulsed) electro-chemical detector

EDL Electrodeless discharge lamp

EDS Energy dispersive spectroscopy

EDTA Ethylenediaminetetraacetic acid

EEC European Economic Community

EFSA European Food Safety Authority

EI Electron impact ionization

EIE Easily ionized elements

ELCD Electrolytic conductivity detector

ELISA Enzyme-linked immunosorbent assay

EM Electron microscopy

EPA Environmental Protection Agency

EPSPS 5-Enolpyruvylshikimate-3-phosphate

synthase

Eq Equivalents

ERH Equilibrium relative humidity

ES Electrospray

E-SEM Environmental scanning electron

microscopy

ESI Electrospray ionization

ESI Electrospray interface

ETD Electron transfer dissociation

ETO Ethylene oxide

EU European Union

Fab Fragment antigen-binding

FAIMS Field-asymmetric ion mobility

FAME Fatty acid methyl esters

FAO/WHO Food and Agricultural Organization/

World Health Organization

FAS Ferrous ammonium sulfate

FBs Fumonisins

Fc Fragment crystallizable

FCC Food Chemicals Codex

FD&C Food, Drug, and Cosmetic

FDA Food and Drug Administration

FDAMA Food and Drug Administration

Modernization Act

FDNB 1-Fluoro-2,4-dinitrobenzene

FFA Free fatty acid

FID Free induction decay

FID Flame ionization detector

FIFRA Federal Insecticide, Fungicide, and

Rodenticide Act

FNB/NAS Food and Nutrition Board of the

National Academy of Sciences

FOS Fructooligosaccharide

FPA Focal plane array

FPD Flame photometric detector

FPIA Fluorescence polarization immunoassay

FPLC Fast protein liquid chromatography

FRAP Ferric reducing antioxidant power

FSIS Food Safety and Inspection Service

FT Fourier transform

FTC Federal Trade Commission

FT-ICR Fourier transform ion cyclotron

resonance

FTIR Fourier transform infrared

FTMS Fourier transform mass spectrometry

G6PDH Glucose-6-phosphate dehydrogenase

GATT General Agreement on Tariffs and

Trade

GC Gas chromatography

GC-AED Gas chromatography-atomic emission

detector

GC-FTIR Gas chromatography-Fourier transform

infrared

GC×GC Comprehensive two-dimensional gas

chromatography

GC-MS Gas chromatography-mass spectrome￾try

GC-O Gas chromatography-olfactory

GFC Gel-filtration chromatography

GIPSA Grain Inspection, Packers and

Stockyards Administration

GLC Gas-liquid chromatography

GMA Grocery Manufacturers of America

GMO Genetically modified organism

GMP Good manufacturing practices (also

current good manufacturing practice in

manufacturing, packing, or holding

human food)

GOPOD Glucose oxidase/peroxidase

GPC Gel-permeation chromatography

GRAS Generally recognized as safe

HACCP Hazard analysis and critical control

point

HAT Hydrogen atom transfer

HCL Hollow cathode lamp

viii Abbreviations

HETP Height equivalent to a theoretical plate

HFS High fructose syrup

HIC Hydrophobic interaction

chromatography

HILIC Hydrophilic interaction liquid

chromatography

HIS Hyperspectral imaging

HK Hexokinase

H-MAS High-resolution magic angle spinning

HMDS Hexamethyldisilazane

HPLC High-performance liquid

chromatography

HPTLC High-performance thin-layer

chromatography

HQI Hit quality index

HRGC High-resolution gas chromatography

HRMS High-resolution accurate mass

spectrometry

HS Headspace

HVP Hydrolyzed vegetable protein

IC Ion chromatography

IC50 Median inhibition concentration

ICP Inductively coupled plasma

ICP-AES Inductively coupled plasma-atomic

emission spectroscopy

ICP-MS Inductively coupled plasma-mass

spectrometer

ICP-OES Inductively coupled plasma-optical

emission spectroscopy

ID Inner diameter

IDF Insoluble dietary fiber

IDK Insect damaged kernels

IEC Inter-element correction

Ig Immunoglobulin

IgE Immunoglobulin E

IgG Immunoglobulin G

IMS Ion mobility mass spectrometry

IMS Interstate Milk Shippers

InGaAs Indium-gallium-arsenide

IR Infrared

IRMM Institute for Reference Materials and

Measurements

ISA Ionic strength adjustor

ISE Ion-selective electrode

ISFET Ion sensitive field effect transitor

ISO International Organization for

Standardization

IT Ion trap

ITD Ion trap detector

IT-MS Ion trap mass spectrometry

IU International Units

IUPAC International Union of Pure and

Applied Chemistry

JECFA Joint FAO/WHO Expert Committee on

Food Additives

kcal Kilocalorie

KDa Kilodalton

KFR Karl Fischer reagent

KFReq Karl Fischer reagent water equivalence

KHP Potassium acid phthalate

LALLS Low-angle laser light scattering

LC Liquid chromatography

LC-MS Liquid chromatography-mass

spectroscopy

LFS Lateral flow strip

LIMS Laboratory information management

system

LM Light microscopy

LOD Limit of detection

LOQ Limit of quantitation

LTM Low thermal mass

LTP Low-temperature plasma probe

m/z Mass-to-charge ratio

MALDI Matrix-assisted laser desorption ionization

MALDI-TOF Matrix-assisted laser desorption

time-of-flight

MALLS Multi-angle laser light scattering

MAS Magic angle spinning

MASE Microwave-assisted solvent extraction

MCL Maximum contaminant level

MCT Mercury:cadmium:telluride

MDGC Multidimensional gas chromatography

MDL Method detection limit

MDSC™ Modulated Differential Scanning

Calorimeter™

mEq Milliequivalents

MES-TRIS 2-(N-morpholino)ethanesulfonic acid￾tris(hydroxymethyl)aminomethane

MLR Multiple linear regression

MRI Magnetic resonance imaging

MRL Maximum residue level

MRM Multiple-reaction monitoring

MRM Multiresidue method

MS Mass spectrometry (or spectrometer)

MS/MS Tandem MS

Msn Multiple stages of mass spectrometry

MW Molecular weight

NAD Nicotinamide-adenine dinucleotide

NADP Nicotinamide-adenine dinucleotide

phosphate

NADPH Reduced NADP

NCM N-Methyl carbamate

NCWM National Conference on Weights and

Measures

NDL Nutrient Data Laboratory

NFDM Nonfat dry milk

NIR Near-infrared

NIRS Near-infrared spectroscopy

NIST National Institute of Standards and

Technology

NLEA Nutrition Labeling and Education Act

NMFS National Marine Fisheries Service

NMR Nuclear magnetic resonance

Abbreviations ix

NOAA National Oceanic and Atmospheric

Administration

NOAEL No observed adverse effect level

NPD Nitrogen phosphorus detector or

thermionic detector

NSSP National Shellfish Sanitation Program

NVC Nonvolatile compounds

NVOC Nonvolatile organic compounds

OC Organochlorine

OD Outer diameter

ODS Octadecylsilyl

OES Optical emission spectroscopy

OMA Official Methods of Analysis

OP Organophosphate/organophosphorus

OPA O-Phthalaldehyde

ORAC Oxygen radical absorbance capacity

ORAC Optimized Rowland circle alignment

OSI Oil stability index

OT Orbitrap

OTA Ochratoxin A

PAD Pulsed-amperometric detector

PAGE Polyacrylamide gel electrophoresis

PAM I Pesticide Analytical Manual, Volume I

PAM II Pesticide Analytical Manual, Volume II

Pc Critical pressure

PCBs Polychlorinated biphenyls

PCR Principal components regression

PCR Polymerase chain reaction

PDA Photodiode array

PDCAAS Protein digestibility-corrected amino

acid score

PDMS Polydimethylsiloxane

PEEK Polyether ether ketone

PER Protein efficiency ratio

PFPD Pulsed flame photometric detector

pI Isoelectric point

PID Photoionization detector

PLE Pressurized liquid extraction

PLOT Porous-layer open tabular

PLS Partial least squares

PME Pectin methylesterase

PMO Pasteurized Milk Ordinance

PMT Photomultiplier tube

ppb Parts per billion

PPD Purchase product description

ppm Parts per million

ppt Parts per trillion

PSPD Position-sensitive photodiode detector

PTV Programmed temperature vaporization

PUFA Polyunsaturated fatty acids

PVDF Polyvinylidine difluoride

PVPP Polyvinylpolypyrrolidone

Q Quadrupole mass filter

QA Quality assurance

QC Quality control

qMS Quadruple mass spectrometry

QqQ Triple quadrupole

Q-TOF Quadrupole-time-of-flight

Q-trap Quadruple-ion trap

QuEChERS Quick, easy, cheap, effective, rugged,

and safe

RAC Raw agricultural commodity

RAE Retinol activity equivalents

RASFF Rapid alert system for food and feed

RDA Recommended daily allowance

RDI Reference daily intake

RE Retinol equivalent

Rf Relative mobility

RF Radiofrequency

RF Response factor

RI Refractive index

RIA Radioimmunoassay

Rm Relative mobility

RMCD Rapidly methylated β-cyclodextrin

ROSA Rapid one-step assay

RPAR Rebuttable Presumption Against

Registration

RS Resistant starch

RVA RapidViscoAnalyser

SAFE Solvent-assisted flavor evaporation

SASO Saudi Arabian Standards Organization

SBSE Stir-bar sorptive extraction

SD Standard deviation

SDF Soluble dietary fiber

SDS Sodium dodecyl sulfate

SDS-PAGE Sodium dodecyl sulfate-polyacrylamide

gel electrophoresis

SEC Size-exclusion chromatography

SEM Scanning electron microscopy

SERS Surface-enhanced Raman scattering

SET Single electron transfer

SFC Solid fat content

SFC Supercritical fluid chromatography

SFC-MS Supercritical fluid chromatography￾mass spectrometry

SFE Supercritical fluid extraction

SFE-GC Supercritical fluid extraction-gas

chromatography

SFI Solid fat index

SI International System of Units

SKCS Single kernel characteristics system

SMEDP Standard Methods for the Examination

of Dairy Products

SO Sulfite oxidase

SOP Standard operating procedures

SPDE Solid-phase dynamic extraction

SPE Solid-phase extraction

SPME Solid-phase microextraction

SRF Sample response factor

SRM Standard reference materials

x Abbreviations

SRM Selected-reaction monitoring

SRM Single-residue method

SSD Solid state detector

STOP Swab test on premises

SVC Semi-volatile compounds

SVOC Semi-volatile organic compounds

SXI Soft x-ray imaging

TBA Thiobarbituric acid

TBARS TBA reactive substances

TCA Trichloroacetic acid

TCD Thermal conductivity detector

TCP Tocopherols

TDA Total daily intake

TDF Total dietary fiber

TDU Thermal desorption unit

T-DNA Transfer of DNA

TD-NMR Time domain nuclear magnetic

resonance

TEAC Trolox equivalent antioxidant capacity

TEM Transmission electron microscopies

TEMED Tetramethylethylenediamine

Tg Glass transition temperature

TGA Thermogravimetric analysis

Ti Tumor-inducing

TIC Total ion current

TLC Thin-layer chromatography

TMA Thermomechanical analysis

TMCS Trimethylchlorosilane

TMS Trimethylsilyl

TOF Time-of-flight

TOF-MS Time-of-flight mass spectrometry

TPA Texture profile analysis

TPTZ 2,4,6-Tripiyridyl-s-triazine

TQ Triple quadrupole

TS Total solids

TSQ Triple stage quadrupole

TSS Total soluble solids

TSUSA Tariff Schedules of the United States of

America

TTB Alcohol and Tobacco Tax and Trade

Bureau

TWI Total weekly intake

TWIM Traveling wave

UHPC Ultra-high pressure chromatography

UHPLC Ultra-high performance liquid chroma￾tography

UPLC Ultra-performance liquid

chromatography

US United States

USA United States of America

USCS United States Customs Service

USDA United States Department of

Agriculture

USDC United States Department of Commerce

USP United States Pharmacopeia

UV Ultraviolet

UV-Vis Ultraviolet-visible

Vis Visible

VC Volatile compounds

VOC Volatile organic compounds

WDS Wavelength dispersive x-ray

wt Weight

wwb Wet weight basis

XMT X-ray microtomography

XRD X-ray diffractometer

ZEA Zearalenone

Abbreviations xi

xiii

Preface and Acknowledgments v

Abbreviations vii

Part 1 General Information

1 Introduction to Food Analysis 3

1.1 Introduction 4

1.2 Reasons for Analyzing Foods and Types

of Samples Analyzed 4

1.3 Steps in Analysis 8

1.4 Method Selection 9

1.5 Official Methods 12

1.6 Summary 14

1.7 Study Questions 14

References 15

2 US Government Regulations and International

Standards Related to Food Analysis 17

2.1 Introduction 19

2.2 US Federal Regulations Affecting Food

Composition 19

2.3 Regulations and Recommendations

for Milk 28

2.4 Regulations and Recommendations for

Shellfish 29

2.5 Specifications for Foods Purchased

by Government Agencies 30

2.6 International Standards and Policies 31

2.7 Summary 31

2.8 Study Questions 32

References 32

3 Nutrition Labeling 35

3.1 Introduction 36

3.2 US Food and Drug Administration Food

Labeling Regulations 36

3.3 US Department of Agriculture Food

Labeling Regulations 41

3.4 Summary 42

3.5 Study Questions 42

References 43

4 Evaluation of Analytical Data 45

4.1 Introduction 46

4.2 Measures of Central Tendency 46

4.3 Reliability of Analysis 46

4.4 Curve Fitting: Regression Analysis 52

4.5 Reporting Results 55

4.6 Summary 57

4.7 Study Questions 57

4.8 Practice Problems 58

References 59

5 Sampling and Sample Preparation 61

5.1 Introduction 63

5.2 Selection of Sampling Procedures 64

5.3 Types of Sampling Plans 65

5.4 Sampling Procedures 67

5.5 Preparation of Samples 70

5.6 Summary 74

5.7 Study Questions 74

References 75

Part 2 Spectroscopy and Mass Spectrometry

6 Basic Principles of Spectroscopy 79

6.1 Introduction 80

6.2 Light 80

6.3 Energy States of Matter 82

6.4 Energy-Level Transitions

in Spectroscopy 85

6.5 Summary 87

6.6 Study Questions 88

Resource Materials 88

7 Ultraviolet, Visible, and Fluorescence

Spectroscopy 89

7.1 Introduction 90

7.2 Ultraviolet and Visible Absorption

Spectroscopy 90

7.3 Fluorescence Spectroscopy 101

7.4 Summary 103

7.5 Study Questions 103

7.6 Practice Problems 104

Reference 106

Resource Materials 106

Contents

8 Infrared and Raman Spectroscopy 107

8.1 Introduction 109

8.2 Principles of IR Spectroscopy 109

8.3 Mid-IR Spectroscopy 111

8.4 Near-IR Spectroscopy 116

8.5 Raman Spectroscopy 120

8.6 Handheld and Portable Technology 122

8.7 Summary 123

8.8 Study Questions 125

References 125

9 Atomic Absorption Spectroscopy, Atomic

Emission Spectroscopy, and Inductively

Coupled Plasma-Mass Spectrometry 129

9.1 Introduction 131

9.2 General Principles 131

9.3 Atomic Absorption Spectroscopy 132

9.4 Atomic Emission Spectroscopy 137

9.5 Applications of Atomic Absorption

and Emission Spectroscopy 143

9.6 Inductively Coupled Plasma-Mass

Spectrometry 144

9.7 Comparison of AAS, ICP-OES,

and ICP-MS 145

9.8 Summary 147

9.9 Study Questions 147

9.10 Practice Problems 148

References 150

10 Nuclear Magnetic Resonance 151

10.1 Introduction 152

10.2 Principles of NMR Spectroscopy 152

10.3 NMR Spectrometer 157

10.4 Applications 158

10.5 Summary 162

10.6 Study Questions 162

References 162

Resource Materials 163

11 Mass Spectrometry 165

11.1 Introduction 166

11.2 Instrumentation: The Mass

Spectrometer 166

11.3 Interpretation of Mass Spectra 172

11.4 Gas Chromatography-Mass

Spectrometry 174

11.5 Liquid Chromatography-Mass

Spectrometry 175

11.6 Tandem Mass Spectrometry 175

11.7 High-Resolution Mass Spectrometry

(HRMS) 176

11.8 Applications 177

11.9 Summary 180

11.10 Study Questions 180

References 181

Resource Materials 181

Part 3 Chromatography

12 Basic Principles of Chromatography 185

12.1 Introduction 187

12.2 Extraction 187

12.3 Chromatography 187

12.4 Physicochemical Principles

of Chromatographic Separation 193

12.5 Analysis of Chromatographic

Peaks 202

12.6 Summary 209

12.7 Study Questions 209

References 211

13 High-Performance Liquid

Chromatography 213

13.1 Introduction 214

13.2 Components of an HPLC System 214

13.3 Applications in HPLC 220

13.4 Summary 225

13.5 Study Questions 225

References 226

14 Gas Chromatography 227

14.1 Introduction 229

14.2 Sample Preparation for Gas

Chromatography 229

14.3 Gas Chromatographic Hardware

and Columns 236

14.4 Chromatographic Theory 246

14.5 Applications of GC 249

14.6 Summary 251

14.7 Study Questions 251

References 252

Part 4 Compositional Analysis of Foods

15 Moisture and Total Solids Analysis 257

15.1 Introduction 259

15.2 Moisture Content 261

15.3 Water Activity 277

15.4 Moisture Sorption Isotherms 281

15.5 Summary 283

15.6 Study Questions 284

15.7 Practice Problems 285

References 286

16 Ash Analysis 287

16.1 Introduction 288

16.2 Methods 288

16.3 Comparison of Methods 294

xiv Contents

16.4 Summary 294

16.5 Study Questions 294

16.6 Practice Problems 296

References 297

17 Fat Analysis 299

17.1 Introduction 301

17.2 Solvent Extraction Methods 302

17.3 Nonsolvent Wet Extraction

Methods 307

17.4 Instrumental Methods 308

17.5 Comparison of Methods 309

17.6 Summary 310

17.7 Study Questions 310

17.8 Practice Problems 314

References 314

18 Protein Analysis 315

18.1 Introduction 317

18.2 Nitrogen-Based Methods 318

18.3 Infrared Spectroscopy 322

18.4 Colorimetric Methods 322

18.5 Ultraviolet Absorption Methods

for Proteins and Peptides 325

18.6 Nonprotein Nitrogen

Determination 325

18.7 Comparison of Methods 326

18.8 Special Considerations 326

18.9 Summary 327

18.10 Study Questions 327

18.11 Practice Problems 327

References 330

19. Carbohydrate Analysis 333

19.1 Introduction 334

19.2 Sample Preparation 335

19.3 Total Carbohydrate: Phenol-Sulfuric

Acid Method 340

19.4 Mono- and Oligosaccharides 341

19.5 Polysaccharides 345

19.6 Dietary Fiber 349

19.7 Physical Methods 354

19.8 Summary 356

19.9 Study Questions 356

19.10 Practice Problems 357

References 359

20 Vitamin Analysis 361

20.1 Introduction 362

20.2 Bioassay Methods 365

20.3 Microbiological Assays 366

20.4 Chemical Methods 366

20.5 Comparison of Methods 369

20.6 Summary 369

20.7 Study Questions 369

20.8 Practice Problems 370

References 370

21 Traditional Methods for Mineral Analysis 371

21.1 Introduction 373

21.2 Basic Considerations 374

21.3 Methods 376

21.4 Benchtop Rapid Analyzers for Salt 380

21.5 Comparison of Methods 380

21.6 Summary 381

21.7 Study Questions 381

21.8 Practice Problems 384

References 385

Part 5 Chemical Characterization and Associated

Assays

22 pH and Titratable Acidity 389

22.1 Introduction 391

22.2 Calculation and Conversion

for Neutralization Reactions 391

22.3 pH 392

22.4 Titratable Acidity 396

22.5 Summary 402

22.6 Study Questions 403

22.7 Practice Problems 403

References 405

23. Fat Characterization 407

23.1 Introduction 409

23.2 General Considerations 412

23.3 Methods for Bulk Oils and Fats 412

23.4 Lipid Oxidation: Measuring Present

Status 418

23.5 Lipid Oxidation: Evaluating Oxidative

Stability 421

23.6 Methods for Lipid Components 422

23.7 Summary 426

23.8 Study Questions 427

23.9 Practice Problems 427

References 428

24 Protein Separation and Characterization

Procedures 431

24.1 Introduction 432

24.2 Methods of Protein Separation 432

24.3 Protein Characterization

Procedures 442

24.4 Summary 450

24.5 Study Questions 450

24.6 Practice Problems 452

References 452

Contents xv