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Electrochemical Detection in Hplc

, by Flanagan, Robert J.; Perrett, David; Whelpton, Robin

Electrochemical Detection in Hplc by Flanagan, Robert J.; Perrett, David; Whelpton, Robin, 9780854045327

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ISBN: 9780854045327 | 0854045325
Cover: Hardcover
Copyright: 8/1/2005

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Summary

Table of Contents

Supplemental Materials

Electrochemical Detection in HPLC: Analysis of Drugs and Poisons is the first monograph devoted to the application of this mode of analysis to the assay of exogenous compounds such as drugs in biological fluids and associated areas. The introductory chapters provide information on basic electrochemistry and HPLC-ED, and on trouble-shooting. The specialized area of thiol analysis is also discussed in detail. Salient practical details of published applications of the technique in analytical toxicology and related areas are provided in a standard format. Alternative techniques are suggested throughout. The emphasis is on the analysis of exogenous compounds, although catecholamines and other endogenous species are discussed in so far as they may be used as drugs. The practical nature of this book will make it useful to professionals working in the field. It will also be of benefit to analysts wishing to use HPLC-ED in the analysis of biological samples for analytes not specifically covered in the volume.

List of Abbreviations

xi

Chapter 1 General Introduction

1

(5)

1 Introduction

1

(2)

2 HPLC-ED in Analytical Toxicology

3

(2)

References

5

(1)

Chapter 2 Basic Electrochemistry for the Separation Scientist

6

(15)

1 Reversible Electrode Potentials

6

(3)

1.1 Redox Electrodes

7

(2)

2 Theoretical Background Linking Electrochemistry to Electrochemical Detection

9

(2)

3 Reference Electrodes

11

(2)

3.1 Standard Hydrogen Electrode

11

(1)

3.2 Calomel Electrode

11

(1)

3.3 Silver/Silver Chloride Electrode

12

(1)

4 Voltammetry

13

(3)

4.1 Cyclic Voltammetry

13

(2)

4.2 Hydrodynamic Voltammograms

15

(1)

5 Electroactivity of Functional Groups and Compounds

16

(4)

5.1 Electrochemical Behaviour of Some Specific Molecular Types

18

(2)

References

20

(1)

Further Reading

20

(1)

Chapter 3 The Electrochemical Detector

21

(35)

1 Introduction

21

(1)

2 Theoretical Background to ED in Flowing Liquid Streams

21

(2)

3 The Construction of an Electrochemical Detector

23

(7)

3.1 Principles of Electrochemical Measurement

23

(1)

3.2 Electrode Materials

24

(4)

3.3 Electrode Shielding and Grounding

28

(1)

3.4 Flow-Cell Designs

28

(1)

3.5 Chromatographic Factors Affecting Flow-Cell Design

29

(1)

3.6 Circuitry of an Electrochemical Detector

30

(1)

4 Amperometric Detection

30

(4)

4.1 Thin-Layer Cells

30

(1)

4.2 Wall-Jet Cells

31

(1)

4.3 Dropping Mercury Electrodes

32

(1)

4.4 Operation of Amperometric Electrodes

33

(1)

5 Coulometric Detection

34

(7)

5.1 Modes of Operation

37

(4)

6 Pulsed Detection

41

(2)

7 Multiple Detection Systems

43

(3)

7.1 Array Detectors

43

(2)

7.2 Rapid Scanning Detectors

45

(1)

7.3 Use in Series With Other Detectors

45

(1)

8 Micro-Detectors

46

(3)

8.1 Detectors for Capillary Systems

47

(2)

9 Comparative Performance of EC Detectors

49

(1)

References

50

(6)

Chapter 4 Development and Troubleshooting of HPLC-ED Methods

56

(23)

1 System Optimisation

56

(9)

1.1 Hydrodynamic Voltammograms

57

(2)

1.2 Eluent Composition

59

(3)

1.3 Temperature

62

(1)

1.4 Flow-Rate

63

(1)

1.5 Electrode Surface

63

(1)

1.6 Gradient Elution

64

(1)

2 Analyte-Related Variables

65

(7)

2.1 Electrochemical Oxidation

66

(1)

2.2 Electrochemical Reduction

66

(1)

2.3 Common Interferences in Biofluid Analyses

67

(1)

2.4 Sample Preparation and Choice of Internal Standard

68

(1)

2.5 Derivatisation

69

(2)

2.6 Hydrolysis/Photolysis/Enzymic Reactions

71

(1)

3 Maintenance of HPLC-ED Systems

72

(2)

References

74

(5)

Chapter 5 Thiols, Disulfides and Related Compounds

79

(25)

1 Introduction

79

(3)

1.1 Biologically Important Thiols

79

(1)

1.2 Thiol-Containing Drugs

80

(2)

1.3 Biochemical Background to Thiol Analysis

82

(1)

2 Sample Preparation

82

(2)

2.1 Standard Solutions

82

(1)

2.2 Blood and Tissues

83

(1)

2.3 Urine

83

(1)

3 Measurement of Free Thiols using HPLC-ED

84

(1)

4 Electrochemistry of Thiols

84

(1)

5 Electrochemical Detection of Thiols

85

(5)

5.1 Detection at Mercury Electrodes

85

(1)

5.2 Detection at Gold Amalgam Electrodes

86

(2)

5.3 Detection at Other Solid Electrodes

88

(2)

5.4 Formation of Electroactive Derivatives of Thiols

90

(1)

6 The Electrochemistry of Disulfides and Related Compounds

90

(1)

7 The Electrochemical Detection of Disulfides plus Thiols

90

(5)

7.1 Direct Detection of Disulfides

91

(1)

7.2 Indirect Detection of Disulfides

92

(1)

7.3 In-Series Detection of Disulfides

92

(3)

8 Other Electrochemical Methods for Thiols and/or Disulfides

95

(1)

9 Analysis of Selenium-Containing Compounds

96

(1)

10 Conclusions

96

(1)

References

97

(7)

Chapter 6 Applications of HPLC-ED in the Analysis of Drugs

104

(107)

1 Anaesthetics

104

(2)

2 β2-Adrenergic Agonists

106

(5)

3 Anticancer Drugs

111

(9)

3.1 Alkylating Agents

111

(1)

3.2 Antimetabolites

112

(1)

3.3 Cytotoxic Antibiotics

113

(1)

3.4 Photosensitisers

114

(1)

3.5 Podophyllotoxins

115

(2)

3.6 Vinca Alkaloids

117

(1)

3.7 Miscellaneous Anticancer Drugs

118

(2)

4 Anticholinergics

120

(1)

5 Anticholinesterases

121

(2)

6 Antidepressants

123

(4)

7 Antihistamines

127

(1)

8 Anti-infectives

128

(12)

8.1 Aminoglycoside Antibiotics

129

(1)

8.2 Anti-Folate Drugs

129

(1)

8.3 Antifungals

130

(1)

8.4 Antimalarials

131

(4)

8.5 Antiviral Drugs

135

(1)

8.6 Inhibitors of Bacterial Cell Wall Synthesis

136

(1)

8.7 Macrolide Antibiotics

137

(2)

8.8 Miscellaneous Antibiotics

139

(1)

9 Antimigraine Drugs

140

(1)

10 Antiparkinsonian Drugs

141

(2)

11 Antipsychotics

143

(6)

12 Anxiolytics

149

(1)

13 Cannabinoids

150

(2)

14 Cardiovascular Drugs

152

(11)

14.1 β-Adrenoceptor Antagonists

152

(3)

14.2 Calcium Channel Blockers

155

(3)

14.3 Sympathomimetics

158

(2)

14.4 Other Anti-Hypertensive Agents

160

(1)

14.5 Antiarrhythmic Agents

161

(1)

14.6 Angiotensin-Converting Enzyme Inhibitors

162

(1)

15 Diuretics

163

(2)

16 Non-Opioid Analgesic/Antipyretic/Anti-inflammatory Drugs

165

(3)

17 Opioid Agonists and Antagonists

168

(5)

18 Miscellaneous Pharmaceuticals

173

(6)

References

179

(32)

Chapter 7 Applications of HPLC-ED in Toxicology and Related Areas

211

(8)

1 Ammatoxins

211

(1)

2 Aromatic Amines and Nitro-Compounds

211

(1)

3 Algal and Fungal Toxins

212

(1)

4 Pesticides and Related Compounds

213

(2)

5 Veterinary Drug and Other Food Residues

215

(2)

References

217

(2)

Appendix Non-Aqueous Ionic Eluent Systems for Basic Drugs

219

(6)

References

224

(1)

Subject Index

225

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