Contents Preface Acknowledgements xi Introduction xiii 1 What Instrumental Approaches are Available 1 1.1 Ion Sources 1 1.1.1 Electron Ionization 3 1.1.2 Chemical Ionization 4 1.1.3 Atmospheric Pressure Chemical Ionization 6 1.1.4 Electrospray Ionization 8 1.1.5 Atmospheric Pressure Photoionization 11 1.1.6 Matrix-assisted Laser Desorption/Ionization 12 1.2 Mass Analysers 14 1.2.1 Mass Resolution 14 1.2.2 Sector Analysers 15 1.2.3 Quadrupole Analysers 19 1.2.4 Time-of-flight 25 1.3 GC/MS 27 1.3.1 Total Ion Current (TIC) Chromatogram 27 1.3.2 Reconstructed Ion Chromatogram (RIC) 28 1.3.3 Multiple Ion Detection (MID) 29 1.4 LC/MS 29 1.5 MS/MS 30 1.5.1 MS/MS by Double Focusing Instruments 30 1.5.2 MS/MS by Triple Quadrupoles 31 1.5.3 MS/MS by Ion Traps 32 1.5.4 MS/MS by Q-TOF 34 References 34 2 How to Design a Quantitative Analysis 37 2.1 General Strategy 38 2.1.1 Project 41 2.1.2 Sampling 41 2.1.3 Sample Treatment 42 2.1.4 Instrumental Analysis 43 2.1.5 Method Validation 53 References 53 3 How to Improve Specificity 55 3.1 Choice of a Suitable Chromatographic Procedure 56 3.1.1 GC/MS Measurements in Low and High Resolution Conditions 56 3.1.2 LC/ESI/MS and LC/APCI/MS Measurements 61 3.2 Choice of a Suitable Ionization Method 79 3.3 An Example of High Specificity and Selectivity Methods: The Dioxin Analysis 85 3.3.1 Use of High Resolution MID Analysis 85 3.3.2 NICI in the Analysis of Dioxins, Furans and PCBs 93 3.3.3 MS/MS in the Detection of Dioxins, Furans and PCBs 95 3.4 An Example of MALDI/MS in Quantitative Analysis of Polypeptides: Substance P 101 References 106 4 Some Thoughts on Calibration and Data Analysis 107 4.1 Calibration Designs 108 4.2 Homoscedastic and Heteroscedastic Data 108 4.2.1 Variance Model 109 4.3 Calibration Models 109 4.3.1 Unweighted Regression 109 4.3.2 Weighted Regression 119 4.3.3 A Practical Example 126 4.4 Different Approaches to Estimate Detection and Quantification Limits 130 References 132 Index 135 Quantitative Applications of Mass Spectrometry
Quantitative Applications of Mass Spectrometry
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