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Handbook of Cyanobacterial Monitoring and Cyanotoxin Analysis

Jussi Meriluoto (Editor), Lisa Spoof (Editor), Geoffrey A. Codd (Editor)
ISBN: 978-1-119-06868-6
576 pages
January 2017
Handbook of Cyanobacterial Monitoring and Cyanotoxin Analysis (1119068681) cover image

Description

A valuable handbook containing reviews, practical methods and standard operating procedures.

  • A valuable and practical working handbook containing introductory and specialist content that tackles a major and growing field of environmental, microbiological and ecotoxicological monitoring and analysis
  • Includes introductory reviews, practical analytical chapters and a comprehensive listing of almost thirty Standard Operating Procedures (SOPs)
  • For use in the laboratory, in academic and government institutions and industrial settings
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Table of Contents

List of Contributors xvii

Preface xxvi

Acknowledgements xxviii

Section I Introduction 1

1 Introduction: Cyanobacteria, Cyanotoxins, Their Human Impact, and Risk Management 3
Geoffrey A. Codd, Jussi Meriluoto, and James S. Metcalf

1.1 Introduction 3

1.2 Cyanotoxins 4

1.3 Exposure Routes, Exposure Media, and At‐Risk Human Activities 6

1.4 Cyanobacterial Blooms and Cyanotoxins in Relation to Human Pressures on Water Resources and Climate Change 7

1.5 Aims of the Handbook 7

References 8

Section II Cyanobacteria 9

2 Ecology of Cyanobacteria 11
Jean‐François Humbert and Jutta Fastner

2.1 Introduction 11

2.2 Environmental Conditions Leading to Cyanobacterial Blooms 12

2.3 Population Dynamics of Cyanobacteria 13

2.4 Spatial Distribution of Cyanobacteria in Freshwater Ecosystems 15

2.5 Ecology of the Production of Toxins by Cyanobacteria 16

2.6 General Conclusions 17

References 17

3 Picocyanobacteria: The Smallest Cell‐Size Cyanobacteria 19
Iwona Jasser and Cristiana Callieri

3.1 Introduction 19

3.2 Records of Toxic Picocyanobacteria 21

3.3 Summary 25

References 26

4 Expansion of Alien and Invasive Cyanobacteria 28
Mikołaj Kokociński, Reyhan Akçaalan, Nico Salmaso, Maya Petrova Stoyneva‐Gärtner, and Assaf Sukenik

4.1 Introduction 28

4.2 Definition of Invasive/Alien Species: Nomenclature Problems 29

4.2.1 Invasive Species Concept in Cyanobacteria 29

4.3 Occurrence of Invasive and Alien Cyanobacteria 31

4.4 Factors Enhancing the Expansion of Alien Cyanobacteria 33

4.5 Impact of Cyanobacterial Invasion on Ecosystem 34

References 36

Section III Sampling, Monitoring and Risk Management 41

5 Health and Safety During Sampling and in the Laboratory 43
Roberta Congestri, James S. Metcalf , Luca Lucentini, and Federica Nigro Di Gregorio

5.1 Introduction 43

5.2 Sampling Safety 43

5.3 Laboratory Safety 44

5.4 Cyanotoxin Production and Application 45

5.5 Contamination due to Equipment, Glassware, and Accidents 45

References 45

6 Basic Guide to Detection and Monitoring of Potentially Toxic Cyanobacteria 46
Nico Salmaso, Cécile Bernard , Jean‐François Humbert, Reyhan Akçaalan, Meriç Albay, Andreas Ballot , Arnaud Catherine, Jutta Fastner , Kerstin Häggqvist, Mária Horecká, Katarzyna Izydorczyk, Latife Köker , Jiří Komárek, Selma Maloufi, Joanna Mankiewicz‐Boczek, James S. Metcalf , Antonio Quesada, Catherine Quiblier , and Claude Yéprémian

6.1 Introduction 47

6.2 Monitoring of Cyanobacteria: Sampling Strategies 48

6.3 Cyanobacterial Identification and Quantification 55

Appendix 6.1 Testing Phytoplankton Distributions: χ2 Test (Pearson Goodness‐of‐Fit Test) 63

References 66

7 Case Studies of Environmental Sampling, Detection, and Monitoring of Potentially Toxic Cyanobacteria 70
Kerstin Häggqvist, Reyhan Akçaalan, Isidora Echenique‐Subiabre, Jutta Fastner , Mária Horecká, Jean‐François Humbert, Katarzyna Izydorczyk, Tomasz Jurczak, Mikołaj Kokociński, Tore Lindholm, Joanna Mankiewicz‐Boczek, Antonio Quesada, Catherine Quiblier, and Nico Salmaso

7.1 Introduction 71

7.2 Shallow Lakes 71

7.3 Deep Lakes 74

7.4 Reservoirs 75

7.5 Rivers 77

7.6 The Baltic Sea 78

7.7 Waterbodies Used for Drinking Water Production 79

References 81

8 New Tools for the Monitoring of Cyanobacteria in Freshwater Ecosystems 84
Jean‐François Humbert and Andrea Törökné

8.1 Introduction 84

8.2 Use of Photosynthetic Pigments for the In Situ Quantification of Cyanobacteria and Other Phytoplankton in Water 85

8.3 Integration of Physicochemical and Fluorescence Sensors in Buoys 86

8.4 New Methods for Automatic Cell Counting in Water Samples 86

References 87

9 Remote Sensing of Cyanobacterial Blooms in Inland, Coastal, and Ocean Waters 89
Peter D. Hunter , Mark W. Matthews , Tiit Kutser , and Andrew N. Tyler

9.1 Introduction 89

9.2 Bio‐optical Properties of Marine and Inland Waters 90

9.3 Platforms and Sensors 91

9.4 Overview of Approaches 92

9.5 Case Study Examples 95

9.6 Future Prospects 96

References 98

10 The Italian System for Cyanobacterial Risk Management in Drinking Water Chains 100
Luca Lucentini, Liliana La Sala , Rossella Colagrossi , and Roberta Congestri

10.1 Introduction 100

10.2 Risk Assessment of Toxic Cyanobacterial Outbreaks in Water for Human Consumption in Italy 101

10.3 Framework of Risk Management of Toxic Cyanobacterial Outbreaks in Water for Human Consumption 102

10.4 Risk Information and Communication 106

References 106

Section IV Toxins and Bioactive/Noxious Compounds from Cyanobacteria 107

11 Microcystins and Nodularins 109
Arnaud Catherine, Cécile Bernard, Lisa Spoof , and Milena Bruno

11.1 Chemical Characteristics and Diversity of Microcystins and Nodularins 109

11.2 Biosynthesis and Genetics of MC and NOD Production 110

11.3 Occurrence of MCs and NODs 112

11.4 Toxicological Effects and Associated Health Risk 113

11.5 Available Methods for the Analysis of MCs and NODs 117

References 118

12 Cylindrospermopsin and Congeners 127
Mikołaj Kokociński, Ana Maria Cameán, Shmuel Carmeli, Remedios Guzmán‐Guillén, Ángeles Jos, Joanna Mankiewicz‐Boczek , James S. Metcalf , Isabel Maria Moreno, Ana Isabel Prieto, and Assaf Sukenik

12.1 Chemical Characteristics of Cylindrospermopsin and Congeners 127

12.2 Genes Involved in CYN Biosynthesis 128

12.3 CYN Producers and Distribution 128

12.4 Toxicity of CYN 129

12.5 The Biological Role of CYN 132

12.6 Degradation of CYN 132

12.7 Available Methods for Determining CYN in Waters 132

References 133

13 Anatoxin‐a, Homoanatoxin‐a, and Natural Analogues 138
Milena Bruno, Olivier Ploux, James S. Metcalf , Annick Mejean, Barbara Pawlik‐Skowronska, and Ambrose Furey

13.1 Introduction 138

13.2 Chemical Structure, Synthesis, and Reactivity 138

13.3 Biosynthesis of ANTX, HANTX, and dihydroANTX 140

13.4 Occurrence and Producing Strains 140

13.5 Toxicity and Pharmacology 141

13.6 Analytical Methodologies 142

References 144

14 Saxitoxin and Analogues 148
Andreas Ballot, Cécile Bernard, and Jutta Fastner

14.1 Introduction 148

14.2 Toxicity of STXs 149

14.3 Occurrence 149

14.4 Genetics and Biosynthesis 150

14.5 Detection Methods 151

14.6 Guidance Values or National Regulations or Recommendations for Managing STXs 152

References 152

15 Anatoxin‐a(S) 155
James S. Metcalf and Milena Bruno

15.1 Chemical Structure of Anatoxin‐a(S) 155

15.2 Biosynthesis 155

15.3 Occurrence and Producing Strains 156

15.4 Toxicology and Pharmacology 156

15.5 Analytical Methods for Determination and Quantification 157

References 158

16 β‐N‐Methylamino‐l‐Alanine and (S)‐2,4‐Diaminobutyric Acid 160
Olivier Ploux, Audrey Combes, Johan Eriksson, and James S. Metcalf

16.1 Historical Overview 160

16.2 Structure, Synthesis, and Molecular Properties 161

16.3 Neurotoxicity 161

16.4 Methods for Identification and Quantification 162

16.5 Occurrence in Cyanobacteria, Plants, and Animals 162

References 163

17 Lipopolysaccharide Endotoxins 165
Sílvia Monteiro, Ricardo Santos, Luděk Bláha, and Geoffrey A. Codd

17.1 Lipopolysaccharide Endotoxins: Structure 165

17.2 Occurrence of LPS Endotoxins 167

17.3 Toxic Effects of LPS Endotoxins 168

17.4 Methods for Determination of LPS Endotoxins 169

References 170

18 Cyanobacterial Retinoids 173
Kunimitsu Kaya and Tomoharu Sano

18.1 Introduction 173

18.2 Detection of Retinoids Produced by Cyanobacteria 174

18.3 Chemistry and Analysis of Retinoids 175

18.4 Malformations by Cyanobacterial Retinoids 176

18.5 Concluding Remarks 176

References 176

19 Other Cyanobacterial Bioactive Substances 179
Tina Elersek, Luděk Bláha, Hanna Mazur‐Marzec, Wido Schmidt, and Shmuel Carmeli

19.1 Introduction 179

19.2 Aeruginosins and Spumigins 182

19.3 Anabaenopeptins 184

19.4 Biogenic Amines 185

19.5 Depsipeptides 186

19.6 Endocrine Disruptors and Novel Tumour Promoters 187

19.7 Lyngbyatoxins and Other Toxins Produced by Lyngbya majuscula 188

19.8 Microginins 189

19.9 Microviridins 189

References 190

20 Taste and Odour Compounds Produced by Cyanobacteria 196
Triantafyllos Kaloudis, Theodoros M. Triantis, and Anastasia Hiskia

20.1 Cyanobacterial Taste and Odour Compounds in Water Resources 196

20.2 Analytical Methods for Taste and Odour Compounds 197

References 199

Section V Screening and Trace Analysis of Cyanotoxins 203

21 Determination of Cyanotoxins by High‐Performance Liquid Chromatography with Photodiode Array 205
Anastasia Hiskia, Lisa Spoof , Triantafyllos Kaloudis, and Jussi Meriluoto

21.1 Introduction: Application of High‐Performance Liquid Chromatography for Different Classes of Cyanotoxins 205

21.2 HPLC of Microcystins and Nodularins 206

21.3 HPLC of Anatoxins 208

21.4 HPLC of Cylindrospermopsin 208

21.5 Advantages and Disadvantages of HPLC‐PDA 208

References 209

22 Determination of Cyanotoxins by High‐Performance Liquid Chromatography with Fluorescence Derivatization 212
James S. Metcalf and Paulo Baptista Pereira

22.1 Principle of the Technique and Why It Is Used for Cyanotoxins 212

22.2 Types of Reactions for Analysing Paralytic Shellfish Toxins Using High‐Performance Liquid Chromatography with Fluorescence Derivatization 213

22.3 Types of Reactions for Analysing β‐N‐Methylamino‐l‐Alanine and Isomers by HPLC‐FLD 216

22.4 Need for Confirmatory Techniques with HPLC‐FLD 216

References 216

23 Liquid Chromatography–Mass Spectrometry 218
Josep Caixach, Cintia Flores, Lisa Spoof , Jussi Meriluoto, Wido Schmidt, Hanna Mazur‐Marzec, Anastasia Hiskia, Triantafyllos Kaloudis, and Ambrose Furey

23.1 Introduction 218

23.2 Ion Sources 220

23.3 Types of Mass Analysers 225

23.4 Application of LC‐MS in Cyanotoxin Analyses 233

23.5 Overview of Quantitation: Cyanobacterial Toxins 235

23.6 Ion Suppression/Enhancement Considerations 237

23.7 High‐Resolution Mass Spectrometry (HRMS) 239

23.8 MS Experiments for the Detection of Unknown Cyanotoxins 242

23.9 Performance Criteria of LC‐MS Methods for Identification and Quantification of Cyanotoxins 249

References 251

24 Capillary Electrophoresis of Cyanobacterial Toxins 258
Gábor Vasas

24.1 Basic Theory and Introduction of Capillary Electrophoresis 258

24.2 Selection of Separation Methods 259

24.3 Detection Methods 259

24.4 CE Methods of Cyanobacterial Toxins 260

24.5 Future Perspectives 262

References 262

25 Immunoassays and Other Antibody Applications 263
James S. Metcalf and Geoffrey A. Codd

25.1 Introduction 263

25.2 Production of Antibodies versus Cyanotoxins 264

25.3 Applications of Cyanotoxin Antibodies 264

25.4 Cyanotoxin Localisation and Quantification Using Antibodies 265

25.5 Other Cyanotoxin Antibody‐Related Technologies 265

References 266

26 Protein Phosphatase Inhibition Assays 267
James S. Metcalf , Anastasia Hiskia, and Triantafyllos Kaloudis

26.1 Background and Molecular Mechanism of Protein Phosphatase Inhibition 267

26.2 Classes of Compounds that Inhibit Protein Phosphatases 268

26.3 Effects of Microcystins on Cyanobacterial Protein Phosphatases 268

26.4 The Basis of the PPIA Assay for Microcystins and Its Evolution 268

26.5 Comparison of PPIA with Other Analytical Methods for Microcystins 268

26.6 Commercially Available Kits for Microcystins 269

26.7 Improvements to the PPIA Assay to Make It More Specific to Microcystins 269

26.8 Conclusions about the Effectiveness of the PPIA Assay for Microcystins and Nodularins in Different Matrices 269

References 270

27 Bioassay Use in the Field of Toxic Cyanobacteria 272
Luděk Bláha, Ana Maria Cameán , Valérie Fessard , Daniel Gutiérrez‐Praena , Ángeles Jos , Benjamin Marie , James S. Metcalf , Silvia Pichardo , María Puerto , Andrea Törökné , Gábor Vasas, and Bojana Žegura

27.1 Introduction 272

27.2 Drivers and Objectives for Bioassay Use 273

27.3 Classification and Terminology 274

27.4 Bioassays for the Effect Evaluation 275

27.5 Bioassays for Monitoring 276

27.6 Conclusions and Future Perspectives 278

References 278

28 Molecular Tools for the Detection of Toxigenic Cyanobacteria in Natural Ecosystems 280
Jean‐François Humbert

28.1 Introduction 280

28.2 Molecular Methods for the Monitoring of Potentially Toxic Cyanobacteria 281

28.3 Strengths and Limitation of These Molecular Approaches 282

28.4 Conclusions 282

References 283

Section VI Methodological Considerations 285

29 Method Validation Guidelines for the Analysis of Cyanotoxins 287
Theodoros M. Triantis, Triantafyllos Kaloudis, and Anastasia Hiskia

29.1 Introduction: Method Validation as a Requirement for Laboratory Accreditation 287

29.2 Performance Criteria and Validation Protocols for the Analysis of Cyanotoxins in Environmental Studies 288

29.3 Validation Issues Concerning the Analysis of Cyanotoxins 290

References 291

30 Interpretation, Significance, and Reporting of Results 292
Geoffrey A. Codd, Jutta Fastner , Tore Lindholm, Jussi Meriluoto, and James S. Metcalf

30.1 Introduction 292

30.2 Interpretation and Significance of Results 293

30.3 Reporting of Results and Maximization of Benefits 294

30.4 Examples, Debriefing 294

References 296

31 Lessons from the Užice Case: How to Complement Analytical Data 298
Zorica Svirčev , Damjana Drobac , Nada Tokodi , Dunja Đenić , Jelica Simeunović , Anastasia Hiskia , Triantafyllos Kaloudis , Biljana Mijović , Stamenko Šušak , Mlađan Protić , Milka Vidović , Antonije Onjia , Sonja Nybom , Tamara Važić , Tamara Palanački Malešević , Tamara Dulić , Dijana Pantelić , Marina Vukašinović , and Jussi Meriluoto

31.1 Introduction 299

31.2 Vrutci Reservoir and the Cyanobacterial Bloom Detected in December 2013 299

31.3 Analytical Work: Toxin Analyses of Water, Cyanobacterial Biomass, and Fish from Reservoir Vrutci 301

31.4 Complementary Data on Toxicity and Observed Health Problems 302

31.5 Analytical and Supplementary Results Combined: A Plausible Reconstruction of Events in Vrutci Reservoir and the City of Užice 306

31.6 Conclusions from the Užice Case 306

References 307

32 Selection of Analytical Methodology for Cyanotoxin Analysis 309
Jussi Meriluoto , James S. Metcalf and Geoffrey A. Codd

32.1 Introduction 309

32.2 General Comparison of Physicochemical Analyses, Biochemical Methods, and Bioassays 309

32.3 Guidance for Selecting and Using Standard Operating Procedures Found in this Handbook 310

32.4 Methodology versus Required Response Time 311

32.5 Influence of Waterbody History on the Choice of Methods 312

32.6 Integration of the Results Obtained: Making Sense 312

Section VII Standard Operating Procedures (SOPs) 313

SOP 1 Cyanobacterial Samples: Preservation, Enumeration, and Biovolume Measurements 315
Arnaud Catherine, Selma Maloufi, Roberta Congestri, Emanuela Viaggiu, and Renata Pilkaityte

SOP 2 Chlorophyll a Extraction and Determination 331
Claude Yéprémian, Arnaud Catherine, Cécile Bernard, Roberta Congestri, Tina Elersek, and Renata Pilkaityte

SOP 3 Phycocyanin Extraction and Determination 335
Claude Yéprémian, Arnaud Catherine, Cécile Bernard, Roberta Congestri, Tina Elersek, and Renata Pilkaityte

SOP 4 Analysis of Picocyanobacteria Abundance in Epifluorescence Microscopy 339
Iwona Jasser and Cristiana Callieri

SOP 5 Estimation of Cyanobacteria Biomass by Marker Pigment Analysis 343
Jean‐Pierre Descy

SOP 6 Extraction of Cyanotoxins from Cyanobacterial Biomass 350
Leonardo Cerasino, Jussi Meriluoto, Luděk Bláha, Shmuel Carmeli, Triantafyllos Kaloudis, and Hanna Mazur‐Marzec

SOP 7 Solid‐Phase Extraction of Microcystins and Nodularin from Drinking Water 354
Theodoros M. Triantis, Triantafyllos Kaloudis, Sevasti-Kiriaki Zervou, and Anastasia Hiskia

SOP 8 Extraction of Microcystins from Animal Tissues 358
Ondřej Adamovský and Luděk Bláha

SOP 9 Analysis of Microcystins by Online Solid Phase Extraction–Liquid Chromatography Tandem Mass Spectrometry 362
Cintia Flores and Josep Caixach

SOP 10 Determination of Microcystins and Nodularin in Filtered and Drinking Water by LC‐MS/MS 372
Theodoros M. Triantis, Triantafyllos Kaloudis, Sevasti-Kiriaki Zervou, and Anastasia Hiskia

SOP 11 Analysis of Microcystins and Nodularin by Ultra High‐Performance Liquid Chromatography Tandem Mass Spectrometry 379
Leonardo Cerasino

SOP 12 Analysis of Microcystins in Animal Tissues Using LC‐MS/MS 385
Jiří Kohoutek and Luděk Bláha

SOP 13 Quantitative Screening of Microcystins and Nodularin in Water Samples with Commercially Available ELISA Kits 390
Triantafyllos Kaloudis, Theodoros M. Triantis, and Anastasia Hiskia

SOP 14 Quantitative Screening of Microcystins and Nodularin in Water Samples with Commercially Available PPIA Kits 393
Triantafyllos Kaloudis, Theodoros M. Triantis, and Anastasia Hiskia

SOP 15 Solid‐Phase Extraction of Cylindrospermopsin from Filtered and Drinking Water 396
Theodoros M. Triantis, Triantafyllos Kaloudis, and Anastasia Hiskia

SOP 16 Determination of Cylindrospermopsin in Filtered and Drinking Water by LC‐MS/MS 399
Theodoros M. Triantis, Triantafyllos Kaloudis, and Anastasia Hiskia

SOP 17 Solid‐Phase Extraction of Anatoxin‐a from Filtered and Drinking Water 405
Theodoros M. Triantis, Triantafyllos Kaloudis, and Anastasia Hiskia

SOP 18 Determination of Anatoxin‐a in Filtered and Drinking Water by LC‐MS/MS 408
Theodoros M. Triantis, Triantafyllos Kaloudis, and Anastasia Hiskia

SOP 19 Analysis of Anatoxin‐a and Cylindrospermopsin by Ultra High-Performance Liquid Chromatography Tandem Mass Spectrometry 413
Leonardo Cerasino

SOP 20 Extraction and Chemical Analysis of Saxitoxin and Analogues in Water 418
Lutz Imhof and Wido Schmidt

SOP 21 Extraction of BMAA from Cyanobacteria 432
James S. Metcalf, Sandra A. Banack, and Paul A. Cox

SOP 22 Analysis of β-N‐Methylamino‐l‐Alanine by UHPLC‐MS/MS 435
James S. Metcalf, William B. Glover, Sandra A. Banack, and Paul A. Cox

SOP 23 Extraction and LC‐MS/MS Analysis of Underivatised BMAA 439
Elisabeth J. Faassen

SOP 24 Extraction, Purification, and Testing of LPS from Cyanobacterial Samples 447
Lucie Bláhová and Luděk Bláha

SOP 25 Extraction and Chemical Analysis of Planktopeptin and Anabaenopeptins 452
Hanna Mazur‐Marzec, Tina Elersek, and Agata Błaszczyk

SOP 26 Thamnocephalus Test 462
Andrea Törökné

SOP 27 Determination of Geosmin and 2‐Methylisoborneol in Water by HS‐SPME‐GC/MS 469
Triantafyllos Kaloudis, Theodoros M. Triantis, and Anastasia Hiskia

SOP 28 Rapid Analysis of Geosmin and 2‐Methylisoborneol from Aqueous Samples Using Solid‐Phase Extraction and GC‐MS 475
Christine Edwards, Craig McKenzie, Carlos Joao Pestana, Kyari Yates, and Linda A. Lawton

SOP 29 Basic Validation Protocol for the Analysis of Cyanotoxins in Environmental Samples 481
Triantafyllos Kaloudis, Theodoros M. Triantis, and Anastasia Hiskia

Section VIII Appendices 487

Appendix 1 Cyanobacterial Species and Recent Synonyms 489

Appendix 2 Cyanobacteria Associated With the Production of Cyanotoxins 501

Appendix 3 Tables of Microcystins and Nodularins 526

Index 538

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