Quantitative Applications of Mass Spectrometry

Professor Pietro Traldi, Research Executive, National Council of Research, CNR, ISTM Corso Stati Uniti 4 I35127 Padova, Italy Fields of interest include structure and reactivity of gaseous ions; -MS application in environmental and biomedical fields; Development of new analytical methods; Instrumental developments. Pietro Traldi is author of over 500 publications on international journals; he is member of the advisory boards of JMS, MSR, RCM and EMS. He is the promoter and the chairman of the Informal Meeting of Mass Spectrometry.Professor Irma Lavagnini, Associate Professor in Analytical Chemistry, Faculty of Pharmacy. Scientific research focus is Chemical data handlingProfessor Franco Magno, Padua University, Italy, Full Professor of Analytical Chemistry since 1980. Main research areas in electroanalytical techniques; Development and application of the digital simulation techniques to rationalize voltammetric responses; Development and optimization of analytical procedures to determine species of relevant enviromental and/or industrial interest. Dr Roberta Seraglia, National Council of Research, Padova, Italy, Researcher of CNR, Institute of Molecular Sciences and Technologies, Padova. 130 papers published in International Journals and 160 communications at International and National congresses.

"…anyone needing to do serious quantitative work using GC/MS could learn from these authors." (CHOICE, January 2007)

• Preface ixAcknowledgements xiIntroduction xiii1 What Instrumental Approaches are Available 11.1 Ion Sources 11.1.1 Electron Ionization 31.1.2 Chemical Ionization 41.1.3 Atmospheric Pressure Chemical Ionization 61.1.4 Electrospray Ionization 81.1.5 Atmospheric Pressure Photoionization 111.1.6 Matrix-assisted Laser Desorption/Ionization 121.2 Mass Analysers 141.2.1 Mass Resolution 141.2.2 Sector Analysers 151.2.3 Quadrupole Analysers 191.2.4 Time-of-flight 251.3 GC/MS 271.3.1 Total Ion Current (TIC) Chromatogram 271.3.2 Reconstructed Ion Chromatogram (RIC) 281.3.3 Multiple Ion Detection (MID) 291.4 LC/MS 291.5 MS/MS 301.5.1 MS/MS by Double Focusing Instruments 301.5.2 MS/MS by Triple Quadrupoles 311.5.3 MS/MS by Ion Traps 321.5.4 MS/MS by Q-TOF 34References 342 How to Design a Quantitative Analysis 372.1 General Strategy 382.1.1 Project 412.1.2 Sampling 412.1.3 Sample Treatment 422.1.4 Instrumental Analysis 432.1.5 Method Validation 53References 533 How to Improve Specificity 553.1 Choice of a Suitable Chromatographic Procedure 563.1.1 GC/MS Measurements in Low and High Resolution Conditions 563.1.2 LC/ESI/MS and LC/APCI/MS Measurements 613.2 Choice of a Suitable Ionization Method 793.3 An Example of High Specificity and Selectivity Methods: The Dioxin Analysis 853.3.1 Use of High Resolution MID Analysis 853.3.2 NICI in the Analysis of Dioxins, Furans and PCBs 933.3.3 MS/MS in the Detection of Dioxins, Furans and PCBs 953.4 An Example of MALDI/MS in Quantitative Analysis of Polypeptides: Substance P 101References 1064 Some Thoughts on Calibration and Data Analysis 1074.1 Calibration Designs 1084.2 Homoscedastic and Heteroscedastic Data 1084.2.1 Variance Model 1094.3 Calibration Models 1094.3.1 Unweighted Regression 1094.3.2 Weighted Regression 1194.3.3 A Practical Example 1264.4 Different Approaches to Estimate Detection and Quantification Limits 130References 132Index 135