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TitleClinical Applications of Mass Spectrometry: Methods and Protocols
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Table of Contents
                            METHODS IN MOLECULAR BIOLOGY
	Clinical Applications of Mass Spectrometry
	Preface
	Contents
	Contributors
The Evolution of Mass Spectrometry in the Clinical Laboratory
	1 Introduction
	2 Introducing Mass Spectrometry into the Clinical Laboratory
	3 Method Comparison and Standardization
	References
Measurement of Plasma/Serum Acylcarnitines Using Tandem Mass Spectrometry
	1 Introduction
	2 Materials
		2.1 Specimens
		2.2 Reagents
		2.3 Acylcarnitine Standards (see Note 2)
		2.4 Internal Standard Working Solutions
		2.5 Quality Control
		2.6 Instrumentation and Supplies
	3 Methods
		3.1 Sample Preparation
		3.2 Tandem Mass Spectrometry Analysis
		3.3 Processing Results
		3.4 Evaluating Standard Curves and Calculating Response Factors
		3.5 Calculation of Concentration for Quality Control and Unknown Samples
		3.6 Reference Intervals
		3.7 Interpretation
	4 Notes
	References
Comprehensive Determination of Amino Acids for Diagnosis of Inborn Errors of Metabolism
	1 Introduction
	2 Materials
		2.1 Samples
		2.2 Reagents
		2.3 Calibration Standards
		2.4 Working Internal Standard
		2.5 Instruments and Columns
	3 Methods
		3.1 External Calibration
		3.2 Sample Extraction and Butylation
		3.3 LC/MS/MS Operation and Data Acquisition
		3.4 Data Analysis
	4 Notes
	References
Identification and Quantitation of Amphetamine, Methamphetamine, MDMA, Pseudoephedrine, and Ephedrine in Blood, Plasma, and Serum Using Gas Chromatography-Mass Spectrometry (GC/MS)
	1 Introduction
	2 Materials
		2.1 Specimen Collection and Storage
		2.2 Reagents and Solutions
		2.3 Standards and Calibrators
		2.4 Supplies
	3 Methods
		3.1 Preparation of the Samples, Controls, and Calibrators
		3.2 Unextracted Sample
		3.3 Instrument Operating Conditions
		3.4 Data Analysis
	4 Notes
	References
Quantification of Antidepressants Using Gas Chromatography-Mass Spectrometry
	1 Introduction
	2 Materials
		2.1 Reagents
		2.2 Specimens
		2.3 Equipment and Supplies
	3 Methods
		3.1 Agilent Instrument Conditions
		3.2 Thermo-Fisher Instrument Conditions
		3.3 Stepwise Extraction
		3.4 Screening and Quantification
	4 Notes
	References
Quantitation of Argatroban in Plasma Using Liquid Chromatography Electrospray Tandem Mass Spectrometry (UPLC-ESI-MS/MS)
	1 Introduction
	2 Materials
		2.1 Samples
		2.2 Reagents and Buffers
		2.3 Standards and Calibrators
		2.4 Internal Standard and Quality Controls
		2.5 Supplies
		2.6 Equipment
	3 Methods
		3.1 Stepwise Procedure
		3.2 Instrument Operating Conditions
		3.3 Data Analysis
	4 Notes
	References
Quantitation of Amobarbital, Butalbital, Pentobarbital, Phenobarbital, and Secobarbital in Urine, Serum, and Plasma Using Gas Chromatography-Mass Spectrometry (GC-MS)
	1 Introduction
	2 Materials
		2.1 Samples
		2.2 Reagents and Buffers
		2.3 Standards and Calibrators
		2.4 Internal Standard and Quality Controls
		2.5 Supplies
		2.6 Equipment
	3 Methods
		3.1 Stepwise Procedures
		3.2 Instrument Operating Conditions
		3.3 Data Analysis
	4 Notes
	References
Quantitation of Benzodiazepines in Blood and Urine Using Gas Chromatography-Mass Spectrometry (GC-MS)
	1 Introduction
	2 Materials
		2.1 Chemicals, Reagents, and Buffers
		2.2 Preparation of Calibrators (see Note 2)
			2.2.1 Benzodiazepine Assay
			2.2.2 Alprazolam Assay
		2.3 Preparation of Control Samples (see Note 2)
			2.3.1 Benzodiazepine Assay
			2.3.2 Alprazolam Assay
		2.4 Supplies
		2.5 Equipment
	3 Methods
		3.1 Stepwise Procedure (Excluding Alprazolam)
		3.2 Stepwise Procedure (Alprazolam Only)
		3.3 Instrument Operating Conditions
		3.4 Data Analysis
	4 Notes
	References
LC-MS/MS Analysis of 13 Benzodiazepines and Metabolites in Urine, Serum, Plasma, and Meconium
	1 Introduction
	2 Materials
		2.1 Sample Preparation and Solid-Phase Extraction
		2.2 Calibrators and Controls
		2.3 Supplies
		2.4 Equipment
	3 Methods
		3.1 Sample Preparation Meconium Specimens
		3.2 Sample Preparation Urine Specimens
		3.3 Sample Preparation Serum and Plasma Specimens
		3.4 Hydrolysis
		3.5 Solid-Phase Extraction
		3.6 LC-MS/MS analysis
		3.7 Data Analysis
	4 Notes
	References
Simultaneous Determination and Quantification of 12 Benzodiazepines in Serum or Whole Blood Using UPLC/MS/MS
	1 Introduction
	2 Materials
		2.1 Samples
		2.2 Reagents
		2.3 Standards and Calibrators
		2.4 Controls and Internal Standards
		2.5 Supplies
	3 Methods
		3.1 Sample Preparation
		3.2 Liquid Chromatography Conditions
		3.3 Mass Spectrometry
		3.4 Data Analysis
	4 Notes
	References
Determination of Benzoic Acid in Serum or Plasma by Gas Chromatography-Mass Spectrometry (GC/MS)
	1 Introduction
	2 Materials
		2.1 Sample
		2.2 Reagents
		2.3 Standards and Calibrators
		2.4 Internal Standard and Quality Controls
		2.5 Supplies
		2.6 Equipment
	3 Methods
		3.1 Stepwise Procedure
		3.2 Instrument Operating Conditions
		3.3 Data Analysis
	4 Notes
	References
Quantification of Busulfan in Plasma Using Liquid Chromatography Electrospray Tandem Mass Spectrometry (HPLC-ESI-MS/MS)
	1 Introduction
	2 Materials
		2.1 Samples
		2.2 Solvents and Reagents
		2.3 Internal Standards and Standards
		2.4 Calibrators and Controls
		2.5 Analytical Equipment and Supplies
	3 Methods
		3.1 Stepwise Procedure
		3.2 Analysis
	4 Notes
	References
Quantitation of Total 11-Nor-9-Carboxy-Delta 9-Tetrahydrocannabinol in Urine and Blood Using Gas Chromatography-Mass Spectrometry (GC-MS)
	1 Introduction
	2 Materials
		2.1 Samples
		2.2 Reagents
		2.3 Standards and Calibrators
		2.4 Quality Controls and Internal Standard
		2.5 Supplies
		2.6 Equipment
	3 Methods
		3.1 Stepwise Procedure
		3.2 Instrument Operating Conditions
		3.3 Data Analysis
	4 Notes
	References
Quantitation of Cocaine, Benzoylecgonine, Ecgonine Methyl Ester, and Cocaethylene in Urine and Blood Using Gas Chromatography-Mass Spectrometry (GC-MS)
	1 Introduction
	2 Materials
		2.1 Sample
		2.2 Reagents and Buffers
		2.3 Standards and Calibrators
		2.4 Internal Standards and Quality Controls
		2.5 Supplies
		2.6 Equipment
	3 Methods
		3.1 Stepwise Procedure
		3.2 Instrument Operating Conditions
		3.3 Data Analysis
	4 Notes
	References
Identification and Quantitation of Cocaine, Benzoylecgonine, and Cocaethylene in Blood, Serum, and Plasma Using Ultra-Performance Liquid Chromatography Coupled to Tandem Mass Spectrometry (UPLC-MS/MS)
	1 Introduction
	2 Materials
		2.1 Specimens
		2.2 Reagents and Solutions
		2.3 Standards and Calibrators
		2.4 Controls and Internal Standards
		2.5 Supplies and Equipment
	3 Methods
		3.1 Stepwise Standard and Calibration Curve Preparation Procedure
		3.2 Instrument Operating Conditions
		3.3 Data Analysis
	4 Notes
	References
Detection and Quantification of Cocaine and Benzoylecgonine in Meconium Using Solid Phase Extraction and UPLC/MS/MS
	1 Introduction
	2 Materials
		2.1 Specimen
		2.2 Reagents and Solutions
		2.3 Standards and Calibrators
		2.4 Controls and Internal Standards
		2.5 Supplies and Equipment
	3 Methods
		3.1 Stepwise Sample and Calibration Curve Preparation Procedure
		3.2 Solid Phase Extraction
		3.3 Instrument Operating Conditions
	4 Notes
	References
Diagnosis of Creatine Metabolism Disorders by Determining Creatine and Guanidinoacetate in Plasma and Urine
	1 Introduction
	2 Materials
		2.1 Specimen Requirements
		2.2 Reagents
		2.3 Standards and Calibrators
		2.4 Internal Standard and Quality Controls
		2.5 Equipments
	3 Methods
		3.1 Preparation of Plasma Samples
		3.2 Preparation of Urine Samples
		3.3 Sample Preparation for HPLC/MS/MS Analysis
		3.4 Setup for HPLC and Tandem Mass Spectrometer (see Note 4)
		3.5 Data Analysis
		3.6 Result Interpretation
	4 Notes
	References
Broad Spectrum Drug Screening Using Electron-Ionization Gas Chromatography-Mass Spectrometry (EI-GCMS)
	1 Introduction
	2 Materials
		2.1 Reagents and Buffers
		2.2 Library Reference Standards (Calibrators/Calibration)
		2.3 Internal Standard and Quality Control
		2.4 Extraction Tubes
		2.5 Supplies
		2.6 Equipment
	3 Methods
		3.1 Stepwise Procedure
		3.2 Instrument Operating Conditions
		3.3 Data Analysis
	4 Notes
	References
Broad Spectrum Drug Screening Using Liquid Chromatography-Hybrid Triple Quadrupole Linear Ion Trap Mass Spectrometry
	1 Introduction
	2 Materials
		2.1 Reagents and Buffers (see Note 1)
		2.2 Library Reference Standards (see Note 2)
		2.3 Internal Standard and Quality Controls (see Note 1)
		2.4 Supplies
		2.5 Equipment
	3 Methods
		3.1 Stepwise Procedure
		3.2 Instrument Operating Conditions
		3.3 Data Analysis
	4 Notes
	References
High Sensitivity Measurement of Estrone and Estradiol in Serum and Plasma Using LC-MS/MS
	1 Introduction
	2 Materials
		2.1 Samples
		2.2 Reagents and Buffers
		2.3 Calibrators, Standards, and Quality Controls
		2.4 Equipment
		2.5 Supplies
	3 Methods
		3.1 Stepwise Procedure
		3.2 Chromatographic Conditions
		3.3 Mass Spectrometer Conditions
		3.4 Data Analysis
	4 Notes
	References
3-Hydroxy-Fatty Acid Analysis by Gas Chromatography-Mass Spectrometry
	1 Introduction
	2 Materials
		2.1 Samples
		2.2 Native and Stable-Isotope 3-Hydroxy-Fatty Acids
		2.3 Extraction and Derivatization Reagents
		2.4 Cell Culture Media
	3 Methods
		3.1 Serum/Plasma Sample Extraction and Derivatization
		3.2 Samples Other Than Serum or Plasma
			3.2.1 Media Removed from Cell Culture
			3.2.2 Samples from Mice
		3.3 GC/MS Analysis
	4 Notes
	References
Quantitation of Fentanyl in Blood and Urine Using Gas Chromatography-Mass Spectrometry (GC-MS)
	1 Introduction
	2 Materials
		2.1 Chemical, Reagents, and Buffers
		2.2 Preparation of Fentanyl Calibrators (see Note 2)
		2.3 Preparation of Control Samples (see Note 2)
		2.4 Supplies
		2.5 Equipment
	3 Methods
		3.1 Stepwise Procedure for Fentanyl Assay
		3.2 Instrument Operating Conditions
		3.3 Data Analysis
	4 Notes
	References
Determination of Total Homocysteine in Plasma Using Liquid Chromatography Coupled to Tandem Mass Spectrometry (LC/MS/MS)
	1 Introduction
	2 Materials
		2.1 Specimens
		2.2 Reagents
		2.3 Instruments
	3 Methods
		3.1 Instrument Conditions
		3.2 Procedure
	4 Notes
	References
Quantitation of Homovanillic Acid (HVA) and Vanillylmandelic Acid (VMA) in Urine Using Gas Chromatography-Mass Spectrometry (GC/MS)
	1 Introduction
	2 Materials
		2.1 Sample
		2.2 Reagents
		2.3 Standards and Calibrators
		2.4 Internal Standard and Quality Control Samples
		2.5 Supplies
		2.6 Equipment
	3 Methods
		3.1 Stepwise Procedure
		3.2 Instrument Operating Conditions
		3.3 Data analysis
	4 Notes
	References
Quantitation of 17-OH-Progesterone (OHPG) for Diagnosis of Congenital Adrenal Hyperplasia (CAH)
	1 Introduction
	2 Materials
		2.1 Samples
		2.2 Reagents and Buffers
		2.3 Standards and Calibrators
		2.4 Internal Standard
		2.5 Quality Controls
		2.6 Supplies
		2.7 Equipment
	3 Methods
		3.1 Sample Preparation:
		3.2 Solid Phase Extraction
		3.3 Instrument Operating Conditions
		3.4 Data Analysis
	4 Notes
	References
Determination of Hydroxyurea in Serum or Plasma Using Gas Chromatography-Mass Spectrometry (GC-MS)
	1 Introduction
	2 Materials
		2.1 Sample
		2.2 Reagents and Buffers
		2.3 Standards and Calibrators
		2.4 Internal Standard and Quality Controls
		2.5 Supplies
		2.6 Equipment
	3 Methods
		3.1 Stepwise Procedure
		3.2 Instrument Operating Conditions
		3.3 Data Analysis
	4 Notes
	References
Quantitation of Ibuprofen in Blood Using Gas Chromatography-Mass Spectrometry (GC-MS)
	1 Introduction
	2 Materials
		2.1 Sample
		2.2 Reagents and Buffers
		2.3 Standards and Calibrators
		2.4 Internal Standard and Quality Controls
		2.5 Supplies
		2.6 Equipment
	3 Methods
		3.1 Stepwise Procedure
		3.2 Instrument Operating Conditions
		3.3 Data Analysis
	4 Notes
	References
Quantitation of Indomethacin in Serum and Plasma Using Gas Chromatography-Mass Spectrometry (GC-MS)
	1 Introduction
	2 Materials
		2.1 Sample
		2.2 Reagents and Buffers
		2.3 Standards and Calibrators
		2.4 Internal Standard and Quality Controls
		2.5 Supplies
		2.6 Equipment
	3 Methods
		3.1 Stepwise Procedure
		3.2 Instrument Operating Conditions
		3.3 Data Analysis
	4 Notes
	References
Quantitation of Iothalamate in Urine and Plasma Using Liquid Chromatography Electrospray Tandem Mass Spectrometry (HPLC-ESI-MS/MS)
	1 Introduction
	2 Materials
		2.1 Reagents and Buffers
		2.2 Standards and Calibrators
		2.3 Internal Standard and Quality Controls
		2.4 Supplies
		2.5 Equipment
	3 Methods
		3.1 Plasma - Stepwise Procedure
		3.2 Urine - Stepwise Procedure
		3.3 Instrument Operating Conditions
		3.4 Data Analysis
	4 Notes
	References
Identification and Quantitation of Ketamine in Biological Matrices Using Gas Chromatography-Mass Spectrometry (GC-MS)
	1 Introduction
	2 Materials
		2.1 Sample
		2.2 Reagents and Buffers
		2.3 Calibrators/Calibration
		2.4 Internal Standard and Quality Controls
		2.5 Supplies
		2.6 Equipment
	3 Methods
		3.1 Preparation of Tissue Homogenates
		3.2 Stepwise Procedure
		3.3 Instrument Operating Conditions
		3.4 Data Analysis
	4 Notes
	References
Measurement of Filter Paper Bloodspot Lead by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS)
	1 Introduction
	2 Materials
		2.1 Reagents and Buffers
		2.2 Internal Standards
		2.3 Working Aqueous (AQ) Standards: 0.0, 6.25, 12.5, 25.0, and 50.0 mug/dL Standards
		2.4 10.0, 20.0, 30.0, and 40.0 mug/dL Whole Blood Standards
		2.5 Bloodspot Standards: 10.0, 20.0, 30.0, and 40.0 mug lead/dL Whole Blood on Filter Paper
		2.6 Controls
		2.7 Supplies and Equipment
	3 Methods
		3.1 Preparation of Whole Blood Specimens for Measurement Using Aqueous Standards
		3.2 Preparation of Bloodspot Specimens for Measurement Using Bloodspot Standards
		3.3 ICP Measurement of Pb and Tb
		3.4 Data Analysis
		3.5 Repeat Sample Analysis for Bloodspot [Pb] >25 mug/dL
		3.6 Classification of [Pb] Results
	4 Notes
	References
Multiplex Lysosomal Enzyme Activity Assay on Dried Blood Spots Using Tandem Mass Spectrometry
	1 Introduction
	2 Materials
		2.1 Samples: Dried Blood Spot (DBS) Preparation from Venous Whole Blood
		2.2 Reagents and Buffers (see Note 1)
		2.3 Detergent and Inhibitor Solutions
		2.4 Assay Cocktails (see Notes 3, 4, and 5)
		2.5 Calibration Solutions
		2.6 Quality Control Samples
		2.7 Equipment and Supplies
	3 Methods
		3.1 Extraction of Dried Blood Spots
		3.2 Enzymatic Reactions
		3.3 Sample Clean-Up
		3.4 MS-MS Analysis
		3.5 Data Analysis
	4 Notes
	References
Gas Chromatography-Mass Spectrometry Method for the Determination of Methadone and 2-Ethylidene-1,5-Dimethyl-3, 3-Diphenylpyrrolidine (EDDP)
	1 Introduction
	2 Materials
		2.1 Solvents and Chemicals
		2.2 Prepared Reagents
		2.3 Supplies and Analytical Equipment
	3 Methods
		3.1 Preparation of Working Standards, Controls, and Unknown Samples (Each Run)
		3.2 Extraction and Derivatization
		3.3 Analysis
	4 Notes
	References
Liquid Chromatography-Tandem Mass Spectrometry (LC-MS-MS) Method for Monitoring Methotrexate in the Setting of Carboxypeptidase-G2 Therapy
	1 Introduction
	2 Materials
		2.1 Reagents and Solutions
		2.2 Calibrators and Controls
		2.3 Supplies
		2.4 Equipment
	3 Methods
		3.1 Stepwise Procedure
		3.2 Liquid Chromatography Conditions
		3.3 Mass Spectrometry
		3.4 Data Analysis
	4 Notes
	References
Quantitation of Methylmalonic Acid in Serum or Plasma Using Isotope Dilution-Selected Ion Gas Chromatography-Mass Spectrometry
	1 Introduction
	2 Materials
		2.1 Reagents
		2.2 Working Reagents
	3 Methods
		3.1 Stepwise Procedure
		3.2 Gas Chromatography Conditions
		3.3 Data Acquisition and Analysis
		3.4 Quality Control, Proficiency Testing
		3.5 Reference Values, Analytical Measurement Range, and Clinical Reportable Range
	References
Quantitation of Methylmalonic Acid in Plasma Using Liquid Chromatography - Tandem Mass Spectrometry
	1 Introduction
	2 Materials
		2.1 Reagents and Buffers
		2.2 Calibrators/Calibration
		2.3 Internal Standard and Quality Controls
		2.4 Tune Solution
		2.5 Supplies
		2.6 Equipment
	3 Methods
		3.1 Stepwise Procedure
		3.2 Instrument Operating Conditions
		3.3 Data Analysis
	4 Notes
	References
Monitoring of Mycophenolate Acid in Serum or Plasma Using LC Tandem Mass Spectrometry
	1 Introduction
	2 Materials
		2.1 Samples
		2.2 Reagents
		2.3 Calibrators
		2.4 Controls
		2.5 Equipment and Supplies
	3 Method
		3.1 Stepwise Procedure
		3.2 Chromatography and Mass Spectrometry Conditions
		3.3 Analysis
	4 Notes
	References
Quantitation of Nicotine, Its Metabolites, and Other Related Alkaloids in Urine, Serum, and Plasma Using LC-MS-MS
	1 Introduction
	2 Materials
		2.1 Specimens
		2.2 Reagents
		2.3 Calibrators
		2.4 Internal Standard Solutions
		2.5 Quality Control Materials
		2.6 Equipment and Supplies
	3 Methods
		3.1 Stepwise Procedure
		3.2 LC Conditions
		3.3 MS Settings
		3.4 Data Analysis
	4 Notes
	References
Quantitation of Opioids in Blood and Urine Using Gas Chromatography-Mass Spectrometry (GC-MS)
	1 Introduction
	2 Materials
		2.1 Chemical, Reagents, and Buffers
		2.2 Preparation of Calibrators (see Note 2)
			2.2.1 Opioid Assay (Morphine, Codeine, Hydromorphone, and Hydrocodone)
			2.2.2 6-Acetylmorphine Assay
		2.3 Preparation of Control Samples (see Note 2)
			2.3.1 Opioid Assay (Morphine, Codeine, Hydromorphone, and Hydrocodone)
			2.3.2 6-Acetylmorphine Assay
		2.4 Supplies
		2.5 Equipment
	3 Methods
		3.1 Stepwise Procedure for Opioid Assay (Morphine, Codeine, Hydromorphone, and Hydrocodone)
		3.2 Stepwise Procedure for 6-Acetylmorphine Assay
		3.3 Instrument Operating Conditions
		3.4 Data Analysis
	4 Notes
	References
Quantitation of Morphine, Codeine, Hydrocodone, Hydromorphone, Oxycodone, Oxymorphone, and 6-Monoacetylmorphine (6-MAM) in Urine, Blood, Serum, or Plasma Using Liquid Chromatography with Tandem Mass Spectrometry Detection
	1 Introduction
	2 Materials
		2.1 Samples
		2.2 Reagents and Buffers
		2.3 Quality Control (QC) Material (see Note 3)
		2.4 Standards and Calibrators
		2.5 Internal Standards
		2.6 Supplies
	3 Methods
		3.1 Urine Samples Preparation
		3.2 Blood Samples Preparation
		3.3 Instrument Operating Conditions
		3.4 Data Analysis
	4 Notes
	References
Urine Organic Acid Analysis for Inherited Metabolic Disease Using Gas Chromatography-Mass Spectrometry
	1 Introduction
	2 Materials
		2.1 Samples
		2.2 Reagents
		2.3 Quality Control Samples
		2.4 Equipment and Supplies
	3 Methods
		3.1 Stepwise Procedure
		3.2 GC-MS Operating Conditions
		3.3 Data Analysis and Interpretation
	4 Notes
	References
Identification of Urine Organic Acids for the Detection of Inborn Errors of Metabolism Using Urease and Gas Chromatography-Mass Spectrometry (GC-MS)
	1 Introduction
	2 Materials
		2.1 Samples
		2.2 Reagents and Solutions
		2.3 Standards and Calibrators
		2.4 Internal Standards and Quality Control
		2.5 Supplies
		2.6 Equipment
	3 Method
		3.1 Sample Preparation
		3.2 Creatinine Determination
		3.3 GC-MS Operating Conditions
		3.4 Data Analysis
	4 Notes
	References
Quantitation of Orotic Acid in Urine Using Isotope Dilution-Selected Ion Gas Chromatography-Mass Spectrometry
	1 Introduction
	2 Materials
		2.1 Specimens
		2.2 Reagents
		2.3 Equipment and Supplies
	3 Methods
		3.1 Stepwise Procedure
		3.2 Gas Chromatography Conditions
		3.3 Data Acquisition and Analysis
		3.4 Quality Control, Proficiency Testing
		3.5 Reference Values, Analytical Measurement Range, and Clinical Reportable Range
	4 Notes
	References
Quantitation of Oxycodone in Blood and Urine Using Gas Chromatography-Mass Spectrometry (GC-MS)
	1 Introduction
	2 Materials
		2.1 Chemical, Reagents, and Buffers
		2.2 Preparation of Calibrators (see Note 2)
		2.3 Preparation of Control Samples (see Note 2)
		2.4 Supplies
		2.5 Equipment
	3 Methods
		3.1 Stepwise Procedure for Oxycodone Assay
		3.2 Instrument Operating Conditions
		3.3 Data Analysis
	4 Notes
	References
Quantitation of Phencyclidine (PCP) in Urine and Blood Using Gas Chromatography-Mass Spectrometry (GC-MS)
	1 Introduction
	2 Materials
		2.1 Sample
		2.2 Reagents and Buffers
		2.3 Standards and Calibrators
		2.4 Internal Standard and Quality Controls
		2.5 Supplies
		2.6 Equipment
	3 Methods
		3.1 Stepwise Procedure
		3.2 Instrument Operating Conditions
		3.3 Data Analysis
	4 Notes
	References
Quantitation of Sirolimus Using Liquid Chromatography-Tandem Mass Spectrometry (LC-MS-MS)
	1 Introduction
	2 Materials
		2.1 Samples
		2.2 Supplies
		2.3 Equipment
		2.4 Chemicals
		2.5 Buffers
		2.6 Standards
		2.7 Quality Control Samples
	3 Methods
		3.1 Stepwise Procedure
		3.2 Instrument Operating Conditions (see Notes 4 and 5).
		3.3 Data Analysis
	4 Notes
	References
Quantitation of Tacrolimus in Whole Blood Using High Performance Liquid Chromatography-Tandem Mass Spectrometry (HPLC-MS-MS)
	1 Introduction
	2 Materials
		2.1 Samples
		2.2 Supplies
		2.3 Equipment
		2.4 Reagents and Buffers
		2.5 Standard Solutions
		2.6 Working Calibrators and Internal Standard
		2.7 Quality Controls
	3 Methods
		3.1 Stepwise Procedure
		3.2 Instrument Operating Conditions/Setup
		3.3 Data Analysis
	4 Notes
	References
Analysis of Testosterone in Serum Using Mass Spectrometry
	1 Introduction
	2 Materials
		2.1 Samples
		2.2 Reagents
		2.3 Calibrators
		2.4 Internal Standards and Quality Control Samples
		2.5 GC-MS Supplies and Equipment
		2.6 LC-MS-MS Supplies and Equipment
	3 Methods
		3.1 Stepwise Procedure for Negative Chemical Ionization GC-MS Analysis of Testosterone
		3.2 GC-MS Conditions
		3.3 Stepwise Procedure for LC-MS-MS Analysis of Testosterone
		3.4 LC-MS-MS Conditions and Data Analysis
	4 Notes
	References
Determination of Tetrahydrozoline in Urine and Blood Using Gas Chromatography-Mass Spectrometry (GC-MS)
	1 Introduction
	2 Materials
		2.1 Sample
		2.2 Reagents
		2.3 Standards and Calibrators
		2.4 Internal Standard and Quality Controls
		2.5 Supplies
		2.6 Equipment
	3 Methods
		3.1 Stepwise Procedure
		3.2 Instrument Operating Conditions
		3.3 Data Analysis
	4 Notes
	References
Quantitation of 25-OH-Vitamin D (25OHD) Using Liquid Tandem Mass Spectrometry (LC-MS-MS)
	1 Introduction
	2 Materials
		2.1 Samples
		2.2 Reagents and Buffers
		2.3 Standards and Calibrators
		2.4 Internal Standard
		2.5 Quality Controls
		2.6 Supplies
		2.7 Equipment
	3 Methods
		3.1 Sample Preparation
		3.2 Solid Phase Extraction
		3.3 Instrument Operating Conditions
		3.4 Data Analysis
	4 Notes
	References
Identification and Quantitation of Zolpidem in Biological Matrices Using Gas Chromatography-Mass Spectrometry (GC-MS)
	1 Introduction
	2 Materials
		2.1 Sample
		2.2 Reagents and Buffers
		2.3 Calibrators/Calibration
		2.4 Internal Standard and Quality Controls
		2.5 Supplies
		2.6 Equipment
	3 Methods
		3.1 Preparation of Tissue Homogenates
		3.2 Stepwise Procedure
		3.3 Instrument Operating Conditions
		3.4 Data Analysis
	4 Notes
	References
Identification and Quantitation of Zopiclone in Biological Matrices Using Gas Chromatography-Mass Spectrometry (GC-MS)
	1 Introduction
	2 Materials
		2.1 Sample
		2.2 Reagents and Buffers
		2.3 Calibrators/Calibration
		2.4 Internal Standard and Quality Controls
		2.5 Supplies
		2.6 Equipment
	3 Methods (3, 4, 5)
		3.1 Preparation of Tissue Homogenates
		3.2 Stepwise Procedure
		3.3 Instrument Operating Conditions
		3.4 Data Analysis
	4 Notes
	References
Subject Index
                        
Document Text Contents
Page 1

M E T H O D S I N M O L E C U L A R B I O L O G Y TM

Series Editor
John M. Walker

School of Life Sciences
University of Hertfordshire

Hatfield, Hertfordshire, AL10 9AB, UK

For other titles published in this series, go to
www.springer.com/series/7651

Page 2

Clinical Applications of Mass
Spectrometry
Methods and Protocols

Edited by

Uttam Garg

Children’s Mercy Hospitals and Clinics, Kansas City, MO, USA

Catherine A. Hammett-Stabler

University of North Carolina, Chapel Hill, NC, USA

Page 263

Table 23.1
Typical performances on an intra-day precision assay during a validation survey

Day 5

Prep. N25
Sample Name
Blank
ClinCal
ClinCheck level 1
ClinCheck level 2

Readings Average (uM)

14.42
9.87
22.45

Readings SD (uM)

0.22
0.13
0.21

Readings Precision %

1.55
1.27
0.92

Prep. N26
Sample Name
Blank
ClinCal
ClinCheck level 1
ClinCheck level 2

Readings Average (uM)

14.40
9.68
22.28

Readings SD (uM)

0.06
0.16
0.38

Readings Precision %

0.44
1.68
1.69

Prep. N27
Sample Name
Blank
ClinCal
ClinCheck level 1
ClinCheck level 2

Readings Average (uM)

14.42
9.74
22.83

Readings SD (uM)

0.15
0.13
0.38

Readings Precision %

1.02
1.31
1.68

Prep. N28
Sample Name
Blank
ClinCal
ClinCheck level 1
ClinCheck level 2

Readings Average (uM)

14.42
9.25
22.35

Readings SD (uM)

0.08
0.12
0.14

Readings Precision %

0.52
1.33
0.68

Prep. N29
Sample Name
Blank
ClinCal
ClinCheck level 1
ClinCheck level 2

Readings Average (uM)

14.40
9.85
22.82

Readings SD (uM)

0.11
0.12
0.38

Readings Precision %

0.76
1.25
1.65

Prep. N30
Sample Name
Blank
ClinCal
ClinCheck level 1
ClinCheck level 2
Intra-day results
ClinCheck level 1
ClinCheck level 2

Readings Average (uM)

14.42
9.51
21.50
Average (uM)
9.65
22.04

Readings SD (uM)

0.21
0.10
0.32
SD (uM)
0.24
0.96

Readings Precision %

1.48
1.06
1.47
Precision %
2.45
4.36

Determination of Total Homocysteine in Plasma 259

Page 264

8. The inter-day precision is 3.2% for the level I quality control
sample with an average value of 9.51 mmol/L (reference value
9.41 mmol/L by LC-UV) and 5.1% for the level II sample
with an average value of 21.91 mmol/L. (reference value
21.7 mmol/L by LC-UV).

References

1. Hanson NQ, Eckfeldt JH, Schwichtenberg
K, Aras O, Tsai MY. Interlaboratory varia-
tion of plasma total homocysteine measure-
ments: results of three successive homo-
cysteine proficiency testing surveys. Clin
Chem. 2002; 48(9):1539–1545.

2. Magera MJ, Lacey JM, Casetta B, Rinaldo P.
Method for the determination of total
homocysteine in plasma and urine by stable
isotope dilution and electrospray tandem
mass spectrometry. Clin Chem. 1999;
45(9):1517–1522.

3. Gempel K, Gerbitz KD, Casetta B, Bauer MF.
Rapid determination of total homocysteine in
blood spots by liquid chromatography-elec-
trospray ionization-tandem mass spectrome-
try. Clin Chem. 2000; 46(1):122–123.

4. Nelson BC, Pfeiffer CM, Sniegoski LT,
Satterfield MB. Development and evalua-
tion of an isotope dilution LC/MS method

for the determination of total homocystine
in human plasma. Anal Chem. 2003;
75:775–784.

5. V. Ducros, Belva-Besnet H, Casetta B,
Favier A. A robust LC/MS/MS method
for total plasma homocysteine determina-
tion in clinical practice. Clin Chem Lab
Med. 2006; 44:987–990.

6. Satterfield MB, Sniegoski LT, Welch MJ,
Nelson BC. Comparison of isotope dilution
mass spectrometry methods for the determi-
nation of total homocysteine in plasma and
serum. Anal Chem. 2003; 75:4631–4638.

7. Tomaiuolo M, Vecchione G, Grandone E,
Cocomazzi N, Casetta B, Di Minno G,
Margaglione M. A new method for determi-
nation of plasma homocystine by isotope
dilution and electrospray tandem mass
spectrometry. J Chromatogr B, 2006;
842:64–69.

Fig. 23.4. Tracings for concentrations approaching the limit of quantitation, estimated in between 0.1 and
0.2 mmol/L.

260 Casetta

Page 526

M

6-MAM..........................................................411–422

Marijuana ...............................................137, 138, 317

Mass spectrometry ........ 1, 2, 3, 5t, 6, 9–24, 28, 37–43,

45–56, 57–62, 65–74, 75–87, 90, 108,

114–115, 121–127, 129–136, 137–143,

145–155, 157–164, 170, 183, 187–201,

203–217, 219, 229–242, 245–251, 253–260,

261–269, 272, 279–286, 289–296, 297–304,

307–314, 317–326, 327–337, 339–350,

351–358, 359–363, 365–369, 371–378,

379–386, 390, 399–410, 411–422, 423–430,

433–443, 445–450, 453–460, 461–467,

469–476, 479–486, 489–499, 501–508,

509–517, 519–526, 527–533

MDMA ................................... 37–43, 191t, 201, 206t

Meconium................................ 89–104, 165–173, 390

Methadone ......... 191t, 197, 199, 206t, 213t, 351–358

Methamphetamine..............................................37–43

Methotrexate ..................................................359–363

3-Methylglutaric acid ................................... 425t, 436t

Methylmalonic acidemia.................................. 16f, 424

Methymalonic acid.......365–369, 371–378, 425t, 428f,

435t, 437, 437t, 441f, 442f

6-MethylUracil ............................................. 425, 425t

Midazolam ............................. 90, 91, 97t, 102t, 103t,

104t, 109, 109t, 110t, 111, 112t, 112t, 113t,

115f, 117t

Mirtazapine ................................47t, 48t, 49t, 52t, 53t

Monoamine oxidase inhibitors ................................. 46

Morphine ............245, 351, 399–402, 404, 406t, 407f,

411–422, 453

Mycophenolate acid ........................................379–386

Mycophenolate mofetil .......................................... 379

N

N-Acetyl – L – Aspartic acid ......................... 425t, 436t

Neuroblastoma ...................................................... 261

Nicotine .........................................................389–397

Non-ketotic hyperglycinemia ................................. 121

Non-steroidal anti-inflammatory drug .............289, 297

11-Nor-delta 9-carboxy-

tetrahydrocannabionol ....................138–142

Nordiazepam.... 76, 77, 79, 84t, 85f, 90, 91, 97t, 102t,

103t, 104t, 109, 109t, 110t, 111, 111t, 113t,

115f, 117t

Nordoxepin ..............................................47t, 52t, 53t

Norepinephrine ............37, 38, 46, 145, 157, 166, 261

Norfluoxetine ....................................47t, 48t, 52t, 53t

Norketamine..............318, 318f, 319, 322, 322t, 323f,

325, 325f

Nornicotine ...................................390, 391, 394f, 396

Nortriptyline..................... 47t, 48t, 49t, 52t, 53t, 213t

O

Opiates ...........................................189, 215, 351, 412

Opioids ......... 189, 245, 247, 351, 399–410, 411, 412,

414, 415, 415t, 417t, 418t, 419t, 420t, 420f,

421f, 453, 455

Opium................................................................... 399

Organic acids ........................ 9, 28, 423–430, 433–443

Ornithine transcarbamylase .................................... 446

Orotic acid................405t, 424, 427t, 436t, 437, 437t,

441f, 445–450

Orotic aciduria........................................445, 446, 450

Oxazepam .. 76, 77, 79, 84t, 85f, 90, 91, 92, 97t, 102t,

103t, 104t, 109, 109t, 110t, 111, 111t, 113t,

115f, 116t, 213t

Oxycodone ....... 191t, 195, 199, 199f, 206t, 213t, 215,

411–422, 453–460

Oxymorphone ........................................411–422, 453

P

Paroxetine .........................................47t, 48t, 52t, 53t

Patent ductus arteriosus ..........................289, 290, 297

Pentobarbital ......................................................65–74

Phencyclidine...... 191t, 201, 206t, 213, 215, 317, 320,

322t, 461–467

Phenobarbital .....................................................65–74

Pheochromocytomas.............................................. 261

Pseudoephedrine ................................................37–43

R

Renal function ..........................57, 280, 298, 307, 360

S

Sebacic acid ....................... 425t, 436t, 437, 437t, 441f

Secobarbital ........................................................65–74

Selective serotonin reuptake inhibitors...................... 46

Sertraline ...........................................47t, 48t, 52t, 53t

Sickle cell ............................................................... 279

Sirolimus ................................................386, 469–476

Steroids ..........................................................272, 276

Suberic acid ................................................. 425t, 435t

Succinylacetone ........................................... 427t, 436t

Switching valve .....136, 207, 222, 223, 223f, 382, 471,

474, 474f, 476, 482, 484, 485f, 486, 499

CLINICAL APPLICATIONS OF MASS SPECTROMETRY 537Subject Index

Page 527

T

Tacrolimus......................................386, 471, 479–486

Temazepam ................................................76, 77, 79,

84t, 85f, 89, 90, 91, 98t, 102t, 103t,

104t, 109, 110t, 111, 111t, 113t, 115f,

116t, 213t

Testosterone...................................................489–499

Tetrahydrocannabinol .....................................137–143

Tetrahydrozoline ............................................501–508

THC ..............................................................137–143

Threoaminobupropion.......................47t, 48t, 52t, 53t

Thrombocytopenia ...................................57, 298, 470

Tiglylglycine ......................................................... 427t

Trans-3’-hydroxy cotinine......................390, 391, 394f

Trazodone..................................47t, 48t, 49t, 52t, 53t

U

Ultra performance liquid chromatography

(UPLC)............. 57–62, 107–119, 157–164,

165–173, 416, 417t, 420f

Urea cycle defects .............................27, 424, 427, 450

V

Vanillylmandelic acid..............................261–269, 436t

Venlafaxine ........................................47t, 48t, 52t, 53t

Vitamin B12 deficiency ...................................366, 371

Vitamin D.......................................................509–517

Z

Zolpidem........................................................519–526

Zopiclone .......................................................527–533

538 CLINICAL APPLICATIONS OF MASS SPECTROMETRYSubject Index

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