Measuring heavy metal contaminants in cannabis and hemp

Cover......Page 1
Half Title......Page 2
Title Page......Page 4
Copyright Page......Page 5
Table of Contents......Page 6
Foreword......Page 18
Preface......Page 22
Acknowledgments......Page 28
Author......Page 34
Chapter 1 The Importance of Testing Cannabis: An Overview of the Analytical Techniques Used......Page 36
 How is Cannabis Being Used?......Page 37
 The Role of Analytical Chemistry......Page 38
 Sampling Protocol for Cannabis in the Field......Page 39
 Heavy Metals and ICP-MS......Page 40
 Pesticides......Page 42
 Potency: Cannabinoids......Page 45
 Terpenes......Page 49
 Residual Solvents......Page 50
 Biological Sample Analysis: Forensic Toxicology......Page 52
 The Determination of THC in the Breath of Motorists......Page 53
 Further Reading......Page 57
Chapter 2 Importance of Measuring Elemental Contaminants in Cannabis and Hemp......Page 60
 Main Factors for Metal Uptake from Soil......Page 61
 Mercury......Page 62
 Cadmium......Page 63
 Cobalt......Page 64
 Vanadium......Page 65
 Other Elements of Concern......Page 66
 Metallic Nanoparticles......Page 67
 State-Based Heavy Metal Limits......Page 68
 Potential of “Real-World” Sources of Elemental Contaminants in Cannabis......Page 71
 Outdoor Growing Sources......Page 72
 Manufacturing/Processing Sources......Page 73
 The Smoking/Inhaling of Cannabis......Page 75
 Laboratory Testing Protocols......Page 76
 A Word about Hemp Regulations......Page 79
 Final Thoughts......Page 80
 Further Reading......Page 81
Chapter 3 What the Cannabis Industry Can Learn from Pharmaceutical Regulations......Page 84
 The Process for Change......Page 85
 USP Implementation Process......Page 86
 Validation Procedures......Page 88
 Toxicity Classification......Page 89
 How are PDEs Calculated?......Page 90
 Cadmium PDE—Oral Exposure......Page 91
 Potential Sources of Elemental Impurities in Drug Compounds......Page 92
 Further Reading......Page 94
 Principles of Operation......Page 96
 Ion Formation......Page 100
 Natural Isotopes......Page 101
 Aerosol Generation......Page 106
 Droplet Selection......Page 108
 Nebulizers......Page 109
 Concentric Design......Page 110
 Microflow Design......Page 111
 Double-Pass Spray Chamber......Page 113
 Cyclonic Spray Chamber......Page 114
 Aerosol Dilution......Page 115
 Further Reading......Page 116
Chapter 7 Plasma Source......Page 118
 The Plasma Torch......Page 119
 The Function of the RF Generator......Page 121
 Ionization of the Sample......Page 123
 Further Reading......Page 124
Chapter 8 Interface Region......Page 126
 Capacitive Coupling......Page 128
 Ion Kinetic Energy......Page 129
 Benefits of a Well-Designed Interface......Page 130
 Final Thoughts......Page 131
 Further Reading......Page 132
 Role of the Ion Optics......Page 134
 Dynamics of Ion Flow......Page 136
 Commercial Ion Optic Designs......Page 137
 Further Reading......Page 140
Chapter 10 Mass Analyzers: Quadrupole Technology......Page 142
 Quadrupole Technology......Page 143
 Quadrupole Performance Criteria......Page 144
  Resolution......Page 145
  Abundance Sensitivity......Page 147
  Benefit of Good Abundance Sensitivity......Page 148
 Further Reading......Page 149
 Magnetic Sector Mass Spectroscopy: A Historical Perspective......Page 150
 Use of Magnetic Sector Technology for ICP-MS......Page 151
 Principles of Operation of Magnetic Sector Technology......Page 152
  Resolving Power......Page 153
 Other Benefits of Magnetic Sector Instruments......Page 154
 Simultaneous Measurement Approach Using One Detector......Page 155
 Further Reading......Page 157
 Basic Principles of TOF Technology......Page 158
 Commercial Designs......Page 159
 Differences between Orthogonal and On-Axis TOF......Page 160
  Rapid Transient Peak Analysis......Page 162
  Rapid Data Acquisition......Page 163
 Laser Ablation Laser Ionization Time-of-Flight Mass Spectrometry......Page 164
 Further Reading......Page 165
Chapter 13 Mass Analyzers: Collision/Reaction Cell and Interface Technology......Page 166
 Basic Principles of Collision/Reaction Cells......Page 167
 Different Collision/Reaction Cell Approaches......Page 168
  Collisional Mechanisms Using Nonreactive Gases and Kinetic Energy Discrimination......Page 169
   Dynamic Reaction Cell......Page 172
   Low Mass Cut-Off Collision/Reaction Cell......Page 175
   “Triple Quadrupole” Collision/Reaction Cell......Page 176
   M/S Mode......Page 178
   Mass Shift MS/MS Mode......Page 179
 The Collision/Reaction Interface......Page 181
 Using Reaction Mechanisms in a Collision Cell......Page 183
 The “Universal” Cell......Page 185
 Final Thoughts......Page 186
 Further Reading......Page 187
Chapter 14 Ion Detectors......Page 190
 Faraday Cup......Page 191
 Discrete Dynode Electron Multiplier......Page 192
  Using Two Scans with One Detector......Page 193
  Using One Scan with One Detector......Page 194
 Extending the Dynamic Range Using Pulse-Only Mode......Page 195
 Simultaneous Array Detectors......Page 196
 Further Reading......Page 198
 Measurement Variables......Page 200
 Measurement Protocol......Page 201
 Optimization of Measurement Protocol......Page 205
 Multielement Data Quality Objectives......Page 206
 Further Reading......Page 211
 Quantitative Analysis......Page 214
  External Standardization......Page 215
  Standard Additions......Page 216
 Semiquantitative Analysis......Page 217
 Isotope Dilution......Page 218
 Internal Standardization......Page 221
 Further Reading......Page 222
 Spectral Interferences......Page 224
 Oxides, Hydroxides, Hydrides, and Doubly Charged Species......Page 225
 Isobaric Interferences......Page 226
 Mathematical Correction Equations......Page 227
 Cool/Cold Plasma Technology......Page 228
 Collision/Reaction Cells......Page 230
 Matrix Interferences......Page 231
 Space Charge-Induced Matrix Interferences......Page 232
 Further Reading......Page 233
Chapter 18 Routine Maintenance......Page 234
 Nebulizers......Page 235
 Spray Chamber......Page 237
 Plasma Torch......Page 238
 Interface Region......Page 239
 Roughing Pumps......Page 241
 Turbomolecular Pumps......Page 242
 Final Thoughts......Page 243
 Further Reading......Page 244
 Sample Preparation Procedures as Described in USP Chapter <233>......Page 246
 Cryogenic Grinding......Page 247
 Collecting the Sample......Page 248
 Typical Sampling Procedures for Cannabis......Page 249
 Digested Sample Weights......Page 250
 Choice of Acids......Page 251
 Digestion Strategies for Cannabis......Page 252
 Rotor-Based Technology......Page 253
 Single Reaction Chamber Technology......Page 255
 Nitrogen-Pressurized Caps......Page 256
 Reagent Blanks......Page 257
 References......Page 258
Chapter 20 Performance and Productivity Enhancement Techniques......Page 260
 Laser Ablation......Page 261
 Excimer Lasers......Page 262
 Benefits of Laser Ablation for ICP-MS......Page 263
 Optimum Laser Design Based on the Application Requirements......Page 264
 193 nm Laser Technology......Page 266
 Flow Injection Analysis......Page 267
 Electrothermal Vaporization (ETV)......Page 271
 Water-Cooled and Peltier-Cooled Spray Chambers......Page 274
 Ultrasonic Nebulizers......Page 275
 Specialized Microflow Nebulizers with Desolvation Techniques......Page 277
 Direct Injection Nebulizers......Page 278
 Productivity Enhancing Techniques......Page 279
 Faster Analysis Times......Page 280
 Automated Sample Identification and Tracking Systems......Page 282
 Further Reading......Page 283
Chapter 21 Coupling ICP-MS with Chromatographic Separation Techniques for Speciation Studies......Page 286
 HPLC Coupled with ICP-MS......Page 288
 Chromatographic Separation Requirements......Page 289
 Ion Exchange Chromatography (IEC)......Page 290
 Column Material......Page 291
 Isocratic or Gradient Elution......Page 292
 Sample Introduction Requirements......Page 293
 Compatibility with Organic Solvents......Page 294
 Collision/Reaction Cell or Interface Capability......Page 295
 Optimization of Peak Measurement Protocol......Page 296
 Full Software Control and Integration......Page 297
 Final Thoughts......Page 298
 Further Reading......Page 299
 Understanding Data Accuracy and Precision......Page 300
 Estimating Error......Page 301
 Types of Errors......Page 302
 Standards and Reference Materials......Page 303
 Using Standards and Reference Materials......Page 304
 Calibration Curves......Page 305
 Laboratory Sources of Error & Contamination......Page 306
 Sources of Laboratory Contamination & Error......Page 309
 Reagents......Page 310
 Laboratory Environment and Personnel......Page 311
 Further Reading......Page 313
Chapter 23 The Importance of Laboratory Quality Assurance......Page 316
 Commercial Reference Materials......Page 317
 Alternate Reference Materials......Page 318
 Quality Assurance Programs......Page 320
 Final Thoughts......Page 321
 Further Reading......Page 322
Chapter 24 Measurement of Elemental Constituents of Cannabis Vaping Liquids and Aerosols by ICP-MS......Page 324
 Vaping Liquid Solvent: The Nature of the Sample......Page 325
 Choice of Liquid Solution Containers......Page 326
 Liquid Sample Containers and Aerosol Collection Materials......Page 328
 Vaping Machines and Trapping Materials......Page 331
 Preparing for Analysis......Page 333
 What Analytes Are Appropriate for Regulatory Purposes?......Page 334
 ICP-MS Instrumentation......Page 335
 Introduction Systems and Optimization......Page 336
 Single Quadrupole-Specific Parameters......Page 337
 “Triple Quadrupole”-Specific Parameters......Page 338
 Further Reading......Page 339
 Basic Definitions......Page 342
 Atomic and Ionic Emission......Page 343
 Sample Introduction......Page 344
 Aerosol Generation......Page 345
 Nebulizers......Page 346
 Spray Chambers......Page 348
 Torches......Page 349
 Fore Optics......Page 351
 Optical Designs......Page 352
 Photomultiplier Tubes......Page 355
 Charge Transfer Devices......Page 356
 Charge-Coupled Devices......Page 357
 Charge-Injection Devices......Page 359
 Analytical Performance......Page 361
 Temperature and Pressure Requirements......Page 362
 Dependence on Plasma Operating Conditions......Page 363
 RF Power......Page 364
 Plasma Gases......Page 365
 Pump Settings......Page 366
 Precision and Accuracy......Page 367
 Detection Limits......Page 368
 Sensitivity......Page 369
 Analytical Wavelength Considerations......Page 370
 Chemical Interferences......Page 372
 Spectral Interferences......Page 374
 Method Validation......Page 376
 Further Reading......Page 377
Chapter 26 Atomic Absorption and Atomic Fluorescence......Page 382
 Flame AAS......Page 383
 FLAAS Interferences and Their Control......Page 384
 Graphite Furnace AAS......Page 386
 GFAAS Interferences and Their Control......Page 388
 Disadvantages of GFAAS......Page 390
 Advantages of Hydride Generation AAS......Page 391
 Atomic Fluorescence......Page 392
 Final Thoughts......Page 393
 Further Reading......Page 394
 X-Ray Fluorescence......Page 396
 XRF Instrumental Configuration......Page 397
 XRF Detection Limits......Page 398
 Laser-Induced Breakdown Spectroscopy......Page 399
 LIBS Fundamental Principles......Page 400
 LIBS on Mars......Page 401
 Microwave-Induced Plasma Optical Emission Spectroscopy......Page 402
 Benefits of MP-AES......Page 403
 Basic Principles LALI-TOFMS......Page 404
 Matrix Effects......Page 405
 Interferences......Page 406
 Operational Use......Page 407
 User Interface......Page 408
 Final Thoughts......Page 409
 Further Reading......Page 410
Chapter 28 What Atomic Spectroscopic Technique is Right for Your Lab?......Page 412
 Flame Atomic Absorption......Page 413
 Atomic Fluorescence......Page 414
 Axial ICP-OES......Page 415
 Comparison Highlights......Page 416
 Demands of the Cannabis Industry......Page 417
 Suitability of Technique......Page 418
 Relationship between LOQ and J-Value......Page 419
 Final Thoughts......Page 420
 Further Reading......Page 421
 Gases......Page 422
 Electricity......Page 423
 Consumables......Page 424
 Cost per Sample......Page 425
 Running Costs of Atomic Fluorescence......Page 426
 Further Reading......Page 427
Chapter 30 How to Select an ICP Mass Spectrometer: Some Important Analytical Considerations......Page 428
 Analytical Performance......Page 429
  Detection Capability......Page 430
  Precision......Page 433
  Isotope Ratio Precision......Page 435
  Accuracy......Page 436
  Dynamic Range......Page 437
  Interference Reduction......Page 439
  Reduction of Matrix-Induced Interferences......Page 445
  Sample Throughput......Page 447
  Single-Particle ICP-MS Transient Signals......Page 449
  Ease of Use......Page 451
  Routine Maintenance......Page 452
  Installation of Instrument......Page 453
 Reliability Issues......Page 454
 Financial Considerations......Page 455
 The Evaluation Process: A Summary......Page 456
 Further Reading......Page 457
 Inductively Coupled Plasma Mass Spectrometry (ICP-MS) Glossary......Page 460
 Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES) Glossary......Page 493
 Atomic Absorption and Atomic Fluorescence......Page 497
 Other Atomic Spectroscopy Techniques......Page 499
Chapter 32 Useful Contact Information......Page 502
Index......Page 514