Statistical designs and response surface techniques for the optimization of chromatographic systems.

This paper describes fundamentals and applications of multivariate statistical techniques for the optimization of chromatographic systems. The surface response methodologies: central composite design, Doehlert matrix and Box-Behnken design are discussed and applications of these techniques for optimization of sample preparation steps (extractions) and determination of experimental conditions for chromatographic separations are presented. The use of mixture design for optimization of mobile phases is also related. An optimization example involving a real separation process is exhaustively described. A discussion about model validation is presented. Some applications of other multivariate techniques for optimization of chromatographic methods are also summarized.

[1]  M. Palma,et al.  Determination of phenolics in cosmetic creams and similar emulsions. , 2005, Journal of Chromatography A.

[2]  D. Massart,et al.  Comparison of the miniaturised techniques capillary electrochromatography and capillary liquid chromatography for the chiral separation of chlorthalidone. , 2004, Journal of pharmaceutical and biomedical analysis.

[3]  G. Saccani,et al.  Determination of acrylamide in drinking water by large-volume direct injection and ion-exclusion chromatography-mass spectrometry. , 2004, Journal of chromatography. A.

[4]  L. Frøyland,et al.  Experimental design considerations in quantification experiments by using the internal standard technique: cholesterol determination by gas chromatography as a case study. , 2006, Journal of chromatography. A.

[5]  M. Peruggia Experiments with Mixtures: Designs, Models, and the Analysis of Mixture Data , 2003 .

[6]  Margaret J. Robertson,et al.  Design and Analysis of Experiments , 2006, Handbook of statistics.

[7]  M. Hows,et al.  Optimisation of a simultaneous separation of sulphonamides, dihydrofolate reductase inhibitors and β-lactam antibiotics by capillary electrophoresis , 1997 .

[8]  Benício de Barros Neto,et al.  25 anos de quimiometria no Brasil , 2006 .

[9]  J. D. De Beer,et al.  Optimization and validation of a micellar electrokinetic chromatographic method for the analysis of several angiotensin-II-receptor antagonists. , 2003, Journal of chromatography. A.

[10]  C. Stalikas,et al.  Development of a method for the simultaneous determination of phosphoric and amino acid group containing pesticides by gas chromatography with mass-selective detection optimization of the derivatization procedure using an experimental design approach. , 2000, Journal of chromatography. A.

[11]  Victor Klee,et al.  Experimental designs through level reduction of the d-dimensional cuboctahedron , 1972, Discret. Math..

[12]  R. Phan-tan-luu,et al.  Experimental design optimization of the analysis of gasoline by capillary gas chromatography , 1997 .

[13]  Remedios Castro Mejías,et al.  Optimisation of headspace solid-phase microextraction for the analysis of volatile phenols in wine. , 2003 .

[14]  大房 健 基礎講座 電気泳動(Electrophoresis) , 2005 .

[15]  Richard F. Gunst,et al.  Applied Regression Analysis , 1999, Technometrics.

[16]  R. Romero,et al.  Optimization of experimental variables in the dabsyl chloride derivatization of biogenic amines for their determination by RP-HPLC , 2000 .

[17]  Peter J. Schoenmakers,et al.  Criteria for optimizing the separation of target analytes in complex chromatograms , 1996 .

[18]  G. R. Hext,et al.  Sequential Application of Simplex Designs in Optimisation and Evolutionary Operation , 1962 .

[19]  C. Pizarro,et al.  Optimisation of a headspace solid-phase microextraction method for the direct determination of chloroanisoles related to cork taint in red wine. , 2004, Journal of chromatography. A.

[20]  L. Frøyland,et al.  Optimisation of an extraction method for the determination of prostaglandin E2 in plasma using experimental design and liquid chromatography tandem mass spectrometry. , 2006, Journal of chromatography. B, Analytical technologies in the biomedical and life sciences.

[21]  M. Petz,et al.  Development of a gas chromatography-mass spectrometry method for the analysis of aminoglycoside antibiotics using experimental design for the optimisation of the derivatisation reactions. , 1998, Journal of chromatography. A.

[22]  R. Cela,et al.  Development of a solid-phase microextraction method for the analysis of phenolic flame retardants in water samples. , 2006, Journal of chromatography. A.

[23]  D. B. Cooper,et al.  Application of central composite design in the optimisation of thermal desorption parameters for the trace level determination of the chemical warfare agent chloropicrin. , 2002, The Analyst.

[24]  S. Rath,et al.  An SPME–GC–MS Method for Determination of Organochlorine Pesticide Residues in Medicinal Plant Infusions , 2005 .

[25]  Erwin Adams,et al.  Evaluation of an International Pharmacopoeia method for the analysis of nelfinavir mesilate by liquid chromatography. , 2006, Journal of chromatography. A.

[26]  D. Steinberg,et al.  Technometrics , 2008 .

[27]  B. Do,et al.  Speciation of arsenic and selenium compounds by ion-pair reversed-phase chromatography with electrothermic atomic absorption spectrometry. Application of experimental design for chromatographic optimisation. , 2001, Journal of chromatography. A.

[28]  R. Poppi,et al.  Simultaneous optimization by neuro-genetic approach of a multiresidue method for determination of pesticides in Passiflora alata infuses using headspace solid phase microextraction and gas chromatography. , 2007, Journal of chromatography. A.

[29]  Á. Garrido-López,et al.  Determination of oleamide and erucamide in polyethylene films by pressurised fluid extraction and gas chromatography. , 2006, Journal of chromatography. A.

[30]  Serge Rudaz,et al.  Optimisation of accelerated solvent extraction of cocaine and benzoylecgonine from coca leaves , 2001 .

[31]  John A. Nelder,et al.  A Simplex Method for Function Minimization , 1965, Comput. J..

[32]  J. J. Carvalho,et al.  Optimization of supercritical fluid extraction of pesticide residues in soil by means of central composite design and analysis by gas chromatography-tandem mass spectrometry. , 2006, Journal of chromatography. A.

[33]  J. H. Ayala,et al.  Optimization of an analytical methodology for the determination of alkyl- and methoxy-phenolic compounds by HS-SPME in biomass smoke , 2006, Analytical and bioanalytical chemistry.

[34]  B. de Barros Neto,et al.  Statistical design--chemometrics , 2006 .

[35]  J. Andrade,et al.  Multivariate optimization and HS-SPME/GC-MS analysis of VOCs in red, yellow and purple varieties of Capsicum chinense sp. peppers , 2006 .

[36]  N. Ferreirós,et al.  Optimization via experimental design of an SPE-HPLC-UV-fluorescence method for the determination of valsartan and its metabolite in human plasma samples. , 2006, Journal of separation science.

[37]  E. Lundanes,et al.  Simultaneous determination of citalopram, fluoxetine, paroxetine and their metabolites in plasma and whole blood by high-performance liquid chromatography with ultraviolet and fluorescence detection. , 1999, Journal of chromatography. B, Biomedical sciences and applications.

[38]  C. Pizarro,et al.  Multiple response optimisation based on desirability functions of a microwave-assisted extraction method for the simultaneous determination of chloroanisoles and chlorophenols in oak barrel sawdust. , 2006, Journal of chromatography. A.

[39]  David H. Doehlert,et al.  Uniform Shell Designs , 1970 .

[40]  R. H. Myers,et al.  Response Surface Methodology: Process and Product Optimization Using Designed Experiments , 1995 .

[41]  D. Westerlund,et al.  Optimization of an HPLC method for the separation of erythromycin and related compounds using factorial design , 1999 .

[42]  R. Cela,et al.  Determination of acidic drugs in sewage water by gas chromatography-mass spectrometry as tert.-butyldimethylsilyl derivatives. , 2003, Journal of chromatography. A.

[43]  G. Derringer,et al.  Simultaneous Optimization of Several Response Variables , 1980 .

[44]  K. Collins,et al.  New stationary phases for high-performance liquid chromatography based on poly(methyltetradecylsiloxane) thermally immobilized onto zirconized silica. , 2006, Journal of chromatography. A.

[45]  J. H. Ayala,et al.  Experimental Design Optimization of Solid‐Phase Microextraction Conditions for the Determination of Heterocyclic Aromatic Amines by High‐Performance Liquid Chromatography , 2006 .

[46]  Marcus Degerman,et al.  Optimisation and robustness analysis of a hydrophobic interaction chromatography step. , 2005, Journal of chromatography. A.

[47]  W. van den Bossche,et al.  Optimization and validation of a capillary zone electrophoretic method for the analysis of several angiotensin-II-receptor antagonists. , 2002, Journal of chromatography. A.

[48]  Ernst Lankmayr,et al.  Screening, optimization and validation of microwave-assisted extraction for the determination of persistent organochlorine pesticides , 2005 .

[49]  M. B. Denton,et al.  Performance of the Super Modified Simplex , 1977 .

[50]  W. Suntornsuk,et al.  Factorial design applied to a non-aqueous capillary electrophoresis method for the separation of beta-agonists. , 2006, Journal of chromatography. A.

[51]  C. Kuo,et al.  Analysis of nine rhubarb anthraquinones and bianthrones by micellar electrokinetic chromatography using experimental design , 2003 .

[52]  P. Araujo A new high performance liquid chromatography multifactor methodology for systematic and simultaneous optimisation of the gradient solvent system and the instrumental/experimental variables , 2000 .

[53]  J. Saurina,et al.  High-performance liquid chromatographic determination of biogenic amines in wines with an experimental design optimization procedure. , 2006, Analytica chimica acta.

[54]  J. Vílchez,et al.  Determination of oxadiazon residues by headspace solid-phase microextraction and gas chromatography-mass spectrometry. , 2002, Journal of chromatography. A.

[55]  M. Guardia,et al.  Microwave-assisted extraction of polybrominated diphenyl ethers and polychlorinated naphthalenes concentrated on semipermeable membrane devices , 2006 .

[56]  Xiaohong Jin,et al.  Development and optimization of organic acid analysis in tobacco with ion chromatography and suppressed conductivity detection. , 2002, Journal of chromatography. A.

[57]  J. Vial,et al.  Robustness study of a reversed-phase liquid chromatographic method for the analysis of carboxylic acids in industrial reaction mixtures. , 2006, Analytica chimica acta.

[58]  Ericka Stricklin-Parker,et al.  Ann , 2005 .

[59]  N. Etxebarria,et al.  Development of a liquid-liquid extraction procedure for five 1,4-dihydropyridines calcium channel antagonists from human plasma using experimental design. , 2005, Talanta.

[60]  S. Benvenuti,et al.  Headspace solid-phase microextraction-gas chromatography--mass spectrometry analysis of the volatile compounds of Evodia species fruits. , 2005, Journal of chromatography. A.

[61]  Desire L. Massart,et al.  Uniform shell designs for optimization in reversed-phase liquid chromatography , 1989 .

[62]  Cristina M Quintella,et al.  Doehlert matrix: a chemometric tool for analytical chemistry-review. , 2004, Talanta.

[63]  A. Seubert,et al.  Application of experimental design for the characterisation of a novel elution system for high-capacity anion chromatography with suppressed conductivity detection. , 1999, Journal of chromatography. A.

[64]  Microemulsion electrokinetic chromatography of drugs varying in charge and hydrophobicity Part II: Strategies for optimization of separation , 2004, Electrophoresis.

[65]  E. Roets,et al.  Development and validation of an improved liquid chromatographic method for the analysis of oxytetracycline , 2002 .

[66]  George E. P. Box,et al.  Empirical Model‐Building and Response Surfaces , 1988 .

[67]  Johanna Smeyers-Verbeke,et al.  Handbook of Chemometrics and Qualimetrics: Part A , 1997 .

[68]  G. G. Stokes "J." , 1890, The New Yale Book of Quotations.

[69]  A. Cifuentes,et al.  Analysis of pesticides in soy milk combining solid-phase extraction and capillary electrophoresis-mass spectrometry. , 2005, Journal of separation science.

[70]  A. Siouffi,et al.  Optimization methods in chromatography and capillary electrophoresis. , 2000, Journal of chromatography. A.

[71]  R. Cela,et al.  Methylmercury determination in biological samples by derivatization, solid-phase microextraction and gas chromatography with microwave-induced plasma atomic emission spectrometry. , 2002, Journal of chromatography. A.

[72]  公庄 庸三 Discrete math = 離散数学 , 2004 .

[73]  Á. Garrido-López,et al.  Determination of 2,4,6-trichloroanisole and guaiacol in cork stoppers by pressurised fluid extraction and gas chromatography-mass spectrometry. , 2006, Journal of chromatography. A.

[74]  Márcia C C Veloso,et al.  Multivariate optimisation of the experimental conditions for determination of three methylxanthines by reversed-phase high-performance liquid chromatography. , 2005, Talanta.

[75]  Yu Ping Zhang,et al.  Rapid separation of Sudan dyes by reverse-phase high performance liquid chromatography through statistically designed experiments. , 2005, Journal of chromatography. A.

[76]  R. Cela,et al.  Multivariate optimization of the factors influencing the solid-phase microextraction of pyrethroid pesticides in water. , 2006, Journal of chromatography. A.

[77]  J. S. Hunter,et al.  Multi-Factor Experimental Designs for Exploring Response Surfaces , 1957 .

[78]  E. Lankmayr,et al.  Screening and optimization of derivatization in heating block for the determination of aliphatic aldehydes by HPLC. , 2006, Journal of biochemical and biophysical methods.

[79]  P. M. Pinheiro,et al.  Detection of 2,4,6-trichloroanisole in chlorinated water at nanogram per litre levels by SPME–GC–ECD , 2005, Analytical and bioanalytical chemistry.

[80]  E. Millán,et al.  Determination of fuel dialkyl ethers and BTEX in water using headspace solid-phase microextraction and gas chromatography-flame ionization detection. , 2004, Journal of chromatography. A.

[81]  Application of multivariate technique in method development for the direct determination of copper in petroleum condensate using graphite furnace atomic absorption spectrometry , 2005 .

[82]  J. Pawliszyn,et al.  Fast and sensitive method to determine chloroanisoles in cork using an internally cooled solid-phase microextraction fiber. , 2007, Journal of chromatography. A.

[83]  Bruce R. Kowalski,et al.  Chemometrics, mathematics and statistics in chemistry , 1984 .

[84]  Douglas C. Montgomery,et al.  Response Surface Methodology: Process and Product Optimization Using Designed Experiments , 1995 .

[85]  F. Safa,et al.  Multi-criteria decision making in micellar liquid chromatographic separation of chlorophenols. , 2004, Journal of separation science.

[86]  D. Thiébaut,et al.  Packed Column SFC of Gas Oils. Part II: Experimental Design Optimization of the Group‐Type Analysis using CO2‐SF6 as the Mobile Phase , 1998 .

[87]  B. Avery,et al.  Development and validation of a stability-indicating reversed-phase high performance liquid chromatography method for NPC 1161C, a novel 8-aminoquinoline anti-malarial drug. , 2006, Journal of chromatography. A.

[88]  C. Turner,et al.  Optimization of a supercritical fluid extraction/reaction methodology for the analysis of castor oil using experimental design. , 2004, Journal of agricultural and food chemistry.

[89]  J. Saurina,et al.  Determination of biogenic amines in wines by ion-pair liquid chromatography and post-column derivatization with 1,2-naphthoquinone-4-sulphonate. , 2006, Journal of chromatography. A.

[90]  Andrew G. Glen,et al.  APPL , 2001 .

[91]  S. D. Jong,et al.  Handbook of Chemometrics and Qualimetrics , 1998 .

[92]  H. Haario,et al.  Optimization of selectivity in high-performance liquid chromatography using desirability functions and mixture designs according to PRISMA. , 1998, European journal of pharmaceutical sciences : official journal of the European Federation for Pharmaceutical Sciences.

[93]  E. Carrilho,et al.  Optimization of solid-phase microextraction procedures for the determination of tricyclic antidepressants and anticonvulsants in plasma samples by liquid chromatography , 2006, Analytical and bioanalytical chemistry.

[94]  M. Abad,et al.  Extraction and quantification of antioxidants from low-density polyethylene by microwave energy and liquid chromatography , 2004 .

[95]  B. Do,et al.  Application of central composite designs for optimisation of the chromatographic separation of monomethylarsonate and dimethylarsinate and of selenomethionine and selenite by ion-pair chromatography coupled with plasma mass spectrometric detection. , 2001, The Analyst.

[96]  Y. Vander Heyden,et al.  Optimisation by experimental design of a capillary electrophoretic method for the separation of several inhibitors of angiotensin-converting enzyme using alkylsulphonates. , 2002, Journal of chromatography. A.

[97]  E. Millán,et al.  Optimization of headspace solid-phase microextraction by means of an experimental design for the determination of methyl tert.-butyl ether in water by gas chromatography-flame ionization detection. , 2002, Journal of chromatography. A.

[98]  Katta G. Murty,et al.  On KΔ , 1986, Discret. Appl. Math..

[99]  T. Mirza,et al.  Determination of captopril in pharmaceutical tablets by anion-exchange HPLC using indirect photometric detection; a study in systematic method development. , 2001, Journal of pharmaceutical and biomedical analysis.

[100]  Josef Havel,et al.  Optimisation of high performance liquid chromatography separation of neuroprotective peptides. Fractional experimental designs combined with artificial neural networks. , 2005, Journal of chromatography. A.

[101]  Á. Garrido-López,et al.  Experimental design approach for the optimisation of pressurised fluid extraction of additives from polyethylene films. , 2005, Journal of chromatography. A.