Robustness of Analytical Chemical Methods and Pharmaceutical Technological Products

, by Hendricks, Margriet M. W. B.; De Boer, Jan H.; Smilde, Age K.; Boer, Jan H. De

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ISBN: 9780444897091 | 0444897097
Cover: Hardcover
Copyright: 11/1/1996

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Chapter 1 GENERAL INTRODUCTION TO ROBUSTNESS

(10)

1.1 INTRODUCTION

(1)

1.2 APPLICATION AREAS AND RELATED ROBUSTNESS QUESTIONS

(2)

1.2.1 Pharmaceutical formulations

(1)

1.2.2 Analytical chemical methods

(1)

1.3 STATISTICAL METHODOLOGY

(4)

1.3.1 Taguchi method

(1)

1.3.2 RSM and Experimental design

(1)

1.3.3 Sequential or simultaneous optimization

(1)

1.3.4 Multicriteria optimization

(1)

1.3.5 Robustness criteria

(1)

1.4 RECOMMENDED READING PATHS

(1)

REFERENCES

(2)

Chapter 2 STABILITY AND RESPONSE SURFACE METHODOLOGY

(68)

2.1 INTRODUCTION

(4)

2.1.1 Example

(2)

2.2 AN OVERVIEW OF RESPONSE SURFACE METHODOLOGY

(20)

2.2.1 First-order designs

(6)

2.2.2 Adding center points

(1)

2.2.3 Second-order designs

(8)

2.2.4 Optimal designs

(1)

2.2.5 Other second-order designs

(1)

2.2.6 Interim Summary

(1)

2.3 ROBUST DESIGN AND RESPONSE SURFACE METHODOLOGY

(22)

2.3.1 Response surface modeling of the mean and standard deviation

(2)

2.3.2 Analyzing the mean and standard deviation response surfaces

(2)

2.3.3 Experimental design with environmental variables

(6)

2.3.4 Analyzing of experimental designs with environmental variables

(6)

2.3.5 Example

(4)

2.4 SPLIT-PLOT DESIGNS FOR ROBUST DESIGN

(16)

2.4.1 Overview of split-plot designs

(10)

2.4.2 Precision of split-plot designs

(1)

2.4.3 Variants of split-plot designs

(1)

2.4.4 Analysis of split-plot designs for robust experimentation

(3)

2.5 CONCLUSIONS

(2)

ACKNOWLEDGEMENTS

(1)

REFERENCES

(4)

Chapter 3 REVIEW OF THE USE OF ROBUSTNESS AND RUGGEDNESS IN ANALYTICAL CHEMISTRY

(70)

3.1 INTRODUCTION

(1)

3.2 PLACE OF RUGGEDNESS TESTING IN METHOD VALIDATION

(3)

3.3 DEFINITIONS OF RUGGEDNESS

(2)

3.4 RUGGEDNESS TESTING OF PROCEDURE RELATED FACTORS

(53)

3.4.1 The steps of a ruggedness test

(1)

3.4.2 Selection of the factors

(2)

3.4.3 Selection of the levels of the factors

(4)

3.4.4 Selection of the experimental design

(20)

3.4.5 Experimental part of the ruggedness test

112

(2)

3.4.6 Analysis of the results

114

(1)

3.4.7 Statistical analysis of the results

115

(9)

3.4.8 Using predefined values to identify chemically relevant factors

124

(3)

3.4.9 Case studies

127

(11)

3.4.10 Expert systems and software packages for ruggedness testing

138

(1)

3.5 RUGGEDNESS TESTING OF NON-PROCEDURE RELATED FACTORS: THE USE OF NESTED DESIGNS

138

(5)

3.6 CONCLUSIONS

143

(1)

ACKNOWLEDGEMENTS

144

(1)

REFERENCES

145

(4)

Chapter 4 ROBUSTNESS CRITERIA; INCORPORATING ROBUSTNESS EXPLICITLY IN OPTIMIZATION PROCEDURES UTILIZING MULTICRITERIA METHODS

149

(42)

4.1 INTRODUCTION

149

(1)

4.2 A BRIEF INTRODUCTION TO THE TAGUCHI METHODS

150

(7)

4.2.1 Introduction

150

(1)

4.2.2 The loss function

151

(3)

4.2.3 Off-line quality control

154

(2)

4.2.4 Orthogonal arrays

156

(1)

4.3 THE ROBUSTNESS CRITERIA

157

(18)

4.3.1 Introduction

157

(2)

4.3.2 The variance/covariance structure of a mixture

159

(7)

4.3.3 General aspects of the robustness criteria

166

(1)

4.3.4 The Jones method

166

(3)

4.3.5 The Weighted Jones method

169

(1)

4.3.6 The Projected Variance method

170

(2)

4.3.7 The Robustness Coefficient

172

(3)

4.4 MULTICRITERIA DECISION MAKING

175

(8)

4.4.1 Introduction

175

(5)

4.4.2 Theory of MCDM

180

(3)

4.5 THE ROBUSTNESS COEFFICIENT APPLIED IN A MCDM STRATEGY

183

(6)

4.5.1 Introduction

183

(1)

4.5.2 Theory

183

(1)

4.5.3 Experimental

184

(1)

4.5.4 Results and discussion

185

(4)

REFERENCES

189

(2)

Chapter 5 RUGGEDNESS TESTS FOR ANALYTICAL CHEMISTRY

191

(42)

5.1 INTRODUCTION

191

(6)

5.1.1 Designing a protocol for method validation

192

(4)

5.1.2 Summary of the role of a ruggedness test in a method validation program

196

(1)

5.2 SELECTION OF FACTORS TO TEST

197

(5)

5.2.1 Selection of the number of levels at which to test a factor

198

(1)

5.2.2 Selection of factors for HPLC methods

198

(3)

5.2.3 Selection of factors for other analytical methods

201

(1)

5.3 SELECTION OF EXPERIMENTAL DESIGNS

202

(12)

5.3.1 Factorial designs

203

(6)

5.3.2 Star designs

209

(2)

5.3.3 Central composite designs

211

(1)

5.3.4 Box-Behnken designs

211

(1)

5.3.5 Matching the ruggedness test to an efficient design

212

(2)

5.4 TREATMENT OF RESULTS

214

(5)

5.4.1 Measurements for a HPLC Study

214

(2)

5.4.2 Treatment of the results from the ruggedness study

216

(1)

5.4.3 Confounding effects in fractional factorial designs

217

(2)

5.5 EXAMPLE CASE STUDIES

219

(11)

5.5.1 The application of a ruggedness test to the assay of Aspirin and its major degradation product, salicylic acid

219

(7)

5.5.2 The application of a ruggedness test to the assay of Salbutamol and its major degradation product, AH4045

226

(4)

5.6 CONCLUSIONS

230

(1)

REFERENCES

230

(3)

Chapter 6 STABILIZING A TLC SEPARATION ILLUSTRATED BY A MIXTURE OF SEVERAL STREET DRUGS

233

(32)

6.1 INTRODUCTION

233

(1)

6.2 THEORY

233

(21)

6.2.1 Thin Layer Chromatography

233

(2)

6.2.2 Separation problem

235

(1)

6.2.3 Selection of mobile phases

236

(2)

6.2.4 Influence of temperature and relative humidity

238

(2)

6.2.5 Optimization

240

(2)

6.2.6 The Taguchi approach to robustness

242

(1)

6.2.7 Application of a parameter design in optimization

243

(2)

6.2.8 Generalization of parameter design towards Response Surface Methodology (RSM)

245

(1)

6.2.9 Construction of experimental designs

246

(2)

6.2.10 Selection of the dependent variable

248

(2)

6.2.11 Construction of models for the dependent variables

250

(1)

6.2.12 Selection criteria for models

251

(1)

6.2.13 Selection of optimization criteria.

252

(2)

6.3 EXPERIMENTAL

254

(1)

6.3.1 Materials and methods

6.3.2 Software

254

(1)

6.4 RESULTS

254

(8)

6.4.1 Introduction

254

(1)

6.4.2 Box Cox transformation

254

(3)

6.4.3 Selection of models

257

(1)

6.4.4 Chromatographic and empirical models

258

(1)

6.4.5 Determination of a solvent with a high minimum resolution

258

(1)

6.4.6 Determination of a solvent composition with a robust minimum resolution

259

(3)

6.5 CONCLUSIONS

262

(1)

REFERENCES

263

(2)

Chapter 7 ROBUSTNESS OF LIQUID-LIQUID EXTRACTION OF DRUGS FROM BIOLOGICAL SAMPLES

265

(44)

7.1 INTRODUCTION

265

(3)

7.2 THEORY

268

(13)

7.2.1 Liquid-liquid extraction optimisation theory

268

(2)

7.2.2 Optimisation criteria

270

(11)

7.3 EXPERIMENTAL

281

(7)

7.3.1 Validation of robustness criteria by means of a comparison with a simulation experiment

281

(3)

7.3.2 Selection of solvents

284

(2)

7.3.3 The extraction of a group of sulphonamides from plasma

286

(2)

7.4 RESULTS AND DISCUSSION

288

(16)

7.4.1 Validation of robustness criteria by means of a comparison with a simulation experiment

288

(7)

7.4.2 The extraction of a group of sulphonamides

295

(9)

7.5 CONCLUSIONS

304

(1)

ACKNOWLEDGEMENTS

305

(1)

REFERENCES

305

(4)

Chapter 8 THE USE OF A FACTORIAL DESIGN TO EVALUATE THE PHYSICAL STABILITY OF TABLETS AFTER STORAGE UNDER TROPICAL CONDITIONS

309

8.1 INTRODUCTION

309

(3)

8.1.1 The use of experimental designs in tablet formulation

310

(1)

8.1.2 The use of factorial designs in physical tablet stability studies

311

(1)

8.2 THE USE OF THE RELATIVE CHANGE IN TABLET PARAMETERS IN A FACTORIAL DESIGN

312

(16)

8.2.1 Planning of the design

313

(1)

8.2.2 Tabletting, storage and measurements

314

(1)

8.2.3 Results

314

(11)

8.2.4 Conclusions

325

(3)

8.3 SELECTION OF EXCIPIENTS SUITABLE FOR USE IN TROPICAL COUNTRIES

328

(12)

8.3.1 Planning of the design

328

(2)

8.3.2 Tabletting, storage and measurements

330

(1)

8.3.3 Results

331

(9)

8.3.4 Conclusions

340

(1)

REFERENCES

340

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Robustness of Analytical Chemical Methods and Pharmaceutical Technological Products

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Supplemental Materials