The analysis of drugs and their metabolites in biological media are now expected to routinely achieve ± 20% accuracy in the ng/mL concentration level. Therefore, the availability and the selection of quality ion-pairs designating the analytes and their isotopically labeled analogs (ILAs) are important considerations in achieving the accuracy of quantitation results. Assisting scientists with this process, Quantitation and Mass Spectrometric Data of Drugs and Isotopically Labeled Analogs provides an extremely valuable reference for labs involved in the analysis of therapeutic and abused drugs. Part One of this comprehensive volume illustrates approaches, mechanisms, and challenges pertaining to the use of isotopic analogs as internal standards for drug quantitation. The second section is a systematic compilation of full-scan mass spectra of drugs and their analogs, as parent compounds and as derivatives resulting from various chemical derivatization approaches, commonly encountered in today’s labs. Based on the mass spectra data presented in the second section, Part Three provides corresponding tables of ion-pairs which can potentially be adapted to designate the drugs and their isotopic analogs in the analytical processes. Relative quality of these ion-pairs (cross-contribution to the intensity of these ions by their isotopic analogs) is included in these tables. With more than 1500 full-scan mass spectra and quick access data tables, this text represents the authors’ years of work compiling mass spectra of the many chemical derivatization forms of drugs, their metabolites, and their isotopically labeled counterparts. The unparalleled scope of this compilation makes it a critical one-stop reference for those involved in drug analyses of biological specimens and interpretation of results.
Author(s): Ray H. Liu, Dennis V. Canfield, Sheng-Meng Wang
Edition: 1
Publisher: CRC Press
Year: 2009
Language: English
Pages: 510
00.pdf......Page 1
Quantitation and Mass Spectrometric Data of Drugs and Isotopically Labeled Analogs......Page 2
Contents......Page 4
Foreword......Page 6
Preface......Page 7
About the Authors......Page 9
PART ONE: ISOTOPICALLY LABELED ANALOG AS INTERNAL STANDARD FOR DRUG QUANTITATION — METHODOLOGY......Page 11
Significance of Accurate Quantitation......Page 12
A. Inadequate Isotopic Purity — An Extrinsic Factor......Page 13
B. Cross-Contribution Derived from Ion Fragmentation Mechanism — An Intrinsic Factor......Page 14
II. FITTING CALIBRATION DATA......Page 15
III. 2H- VERSUS 13C-ANALOGS AS INTERNAL STANDARDS......Page 16
CONCLUDING REMARKS......Page 18
REFERENCES......Page 19
INTRODUCTION......Page 20
B. Exemplar Studies......Page 21
II. ION INTENSITY CROSS-CONTRIBUTION DATA......Page 22
A. Full-Scan Mass Spectra......Page 26
1. Direct Measurement......Page 27
2. Normalized Direct Measurement......Page 28
4. Standard Addition Method......Page 29
C. Assessing the Accuracy of Empirically Determined Cross-Contribution Data......Page 30
1. Empirically Observed Concentration......Page 31
2. Theoretically Calculated Concentration......Page 33
3. Comparing Empirically Observed and Theoretically Calculated Concentrations — Graphic Presentation......Page 34
B. Collection of Mass Spectrometric Data (Appendix One, pp 31–371)......Page 35
C. Ion Intensity Cross-Contribution Data (Appendix Two, pp 373–492)......Page 36
REFERENCES......Page 37
PART TWO: MASS SPECTRA OF COMMONLY ABUSED DRUGS AND THEIR ISOTOPICALLY LABELED ANALOGS IN VARIOUS DERIVATIZATION FORMS......Page 40
Table of Contents for Appendix One......Page 41
Appendix One — Figure I Mass Spectra of Commonly Abused Drugs and Their Isotopically Labeled Analogs in Various Derivatization Forms — Stimulants......Page 43
Appendix One — Figure II Mass Spectra of Commonly Abused Drugs and Their Isotopically Labeled Analogs in Various Derivatization Forms — Opioids......Page 136
Appendix One — Figure III Mass Spectra of Commonly Abused Drugs and Their Isotopically Labeled Analogs in Various Derivatization Forms — Hallucinogens......Page 222
Appendix One — Figure IV Mass Spectra of Commonly Abused Drugs and Their Isotopically Labeled Analogs in Various Derivatization Forms — Depressants/Hypnotics......Page 254
Appendix One — Figure V Mass Spectra of Commonly Abused Drugs and Their Isotopically Labeled Analogs in Various Derivatization Forms — Antianxiety Agents......Page 275
Appendix One — Figure VI Mass Spectra of Commonly Abused Drugs and Their Isotopically Labeled Analogs in Various Derivatization Forms — Antidepressants......Page 327
Appendix One — Figure VII Mass Spectra of Commonly Abused Drugs and Their Isotopically Labeled Analogs in Various Derivatization Forms — Others......Page 347
PART THREE: CROSS-CONTRIBUTIONS OF ION INTENSITY BETWEEN ANALYTES AND THEIR ISOTOPICALLY LABELED ANALOGS IN VARIOUS DERIVATIZATION FORMS......Page 368
Table of Contents for Appendix Two......Page 369
Appendix Two — Table I Cross-Contributions Between ions Designating the Drugs and Their Isotopically Labeled Analogs in Various Derivatization Forms — Stimulants......Page 371
Appendix Two — Table II Cross-Contributions Between ions Designating the Drugs and Their Isotopically Labeled Analogs in Various Derivatization Forms — Opioids......Page 401
Appendix Two — Table III Cross-Contributions Between Ions Designating the Drugs and Their Isotopically Labeled Analogs in Various Derivatization Forms — Hallucinogens......Page 427
Appendix Two — Table IV Cross-Contributions Between ions Designating the Drugs and Their Isotopically Labeled Analogs in Various Derivatization Forms — Depressants/Hypnotics......Page 438
Appendix Two — Table V Cross-Contributions Between Ions Designating the Drugs and Their Isotopically Labeled Analogs in Various Derivatization Forms — Antianxiety Agents......Page 446
Appendix Two — Table VI Cross-Contributions Between Ions Designating the Drugs and Their Isotopically Labeled Analogs in Various Derivatization Forms — Antidepressants......Page 463
Appendix Two — Table VII Cross-Contributions Between Ions Designating the Drugs and Their Isotopically Labeled Analogs in Various Derivatization Forms — Others......Page 469
