Optimisation of chromatographic separations by use of a chromatographic response function, empirical modelling and multivariate analysis

Bylund, Dan; Bergens, Arne; Jacobsson, Sven P.

doi:10.1007/bf02466519

Cited by 27 publications

(14 citation statements)

References 15 publications

Supporting

Mentioning

Contrasting

Unclassified

Order By: Relevance

“…I mix = (J mix /J std )I std (8) where I mix and I std are the concentrations of the analytes in the mixtures and the standard samples, respectively; J mix and J std are the corresponding peak areas.…”

Section: Description Of the Als Methodsmentioning

confidence: 99%

“…When physical separation of sample components is not fully accomplished, quantification difficulties stemming from poorly resolved peaks may still be overcome mathematically using chemometrics [3]. Chemometrics methods have been used in liquid chromatography and other separation techniques to check peak purities [4][5][6], to improve the resolution and quantification [7], and to optimize the separation conditions [8][9][10]. As the applications of CE are widespread in many fields of analytical chemistry, more and more chemometrics methods are modified for CE analysis.…”

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

Quantification of analytes in overlapping peaks from capillary electrophoresis using multivariate curve resolution‐alternating least squares methods

Zhang

Havel

2003

Electrophoresis

View full text Add to dashboard Cite

Application of multivariate curve resolution with alternating least squares (ALS) methods to second-order data from capillary electrophoresis diode array detector (CE-DAD) is shown. Second-order data are easily obtained by setting individual data matrix of CE run one in top of the other. Initial qualitative solutions obtained by evolving factor analysis can be further optimized by simultaneous analysis of multiple electrophoresis run data with ALS regression. Quantification is achieved by the comparison of the analyte peak areas with that of pure standards. During the ALS regression procedure, the following constraints were applied: (i) both concentrations and unit pure spectra of the resolved components must be positive; (ii) elution profiles have an unimodal shape; (iii) correspondence exists between common species in the different data matrices; (iv) the pure spectrum of each species is the same in all runs where it is present. The above methods were applied for the determination of dinitrotoluene (DNT) isomeric compounds in overlapping peaks from CE.

show abstract

Section: Description Of the Als Methodsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Quantification of analytes in overlapping peaks from capillary electrophoresis using multivariate curve resolution‐alternating least squares methods

Zhang

Havel

2003

Electrophoresis

View full text Add to dashboard Cite

show abstract

“…To study the linearity of the response, a series of working standard solutions of 5,10,15,20,25,30,35,40,45 and 50 mg mL -1 for haloperidol and of 0.05, 0.10, 0.15, 0.20, 0.25, 0.30, 0.35, 0.40, 0.45 and 0.50 mg mL -1 for each related compound were prepared. The linearity of peak area response vs. concentration was studied.…”

Section: Validation Proceduresmentioning

confidence: 99%

“…The CRF is a coefficient which characterizes the quality of separation in a quantitative manner. Preferably, a flexible function that allows resolution criteria to be specified (15). The corresponding terms in the chromatogram are then compared to these criteria.…”

Section: Optimization Of Separation Of a Mixture Of Haloperidol And Imentioning

confidence: 99%

Use of chemometrics for development and validation of an RP-HPLC method for simultaneous determination of haloperidol and related compounds

Petkovska¹,

Dimitrovska²

2008

Acta Pharmaceutica

View full text Add to dashboard Cite

Haloperidol is one of the most widely used antipsychotic drugs in the treatment of schizophrenia, mania and other psychiatric disorders (1). Chemically, haloperidol (Hal) is 4-[4-(4-chlorophenyl)-4-hydroxy-1-piperidinyl]-1-(4-fluorophenyl)-1-butanone. The drug has six known related compounds specified as impurities: 4-(4-chlorophenyl)-4-hydroxy A rapid resolution reversed-phase high performance liquid chromatographic (RR RP-HPLC) method has been developed and validated for simultaneous determination of haloperidol and six related compounds. Investigated matrix was a laboratory mixture of a therapeutic active substance haloperidol and its six related compounds in concentration ratio 300:1. Experimental design was used during method optimization (full factorial 2 3 design) and robustness testing (Central Composite Circumscribed design). Three factors: organic phase variation during gradient elution, flow rate and gradient rise time were independent variables. To estimate the system response during the optimization procedure and robustness testing, resolution (R s ) and a chromatographic response function (CRF) were used. Chromatography was performed with the mobile phase containing phosphate buffer pH 6.5 and acetonitrile as organic modifier. Separation was achieved using gradient elution (organic phase fraction changed linearly from 20 to 72 %) over 7 min. A Zorbax Eclipse XDB C18 Rapid Resolution HT 4.6 mm´50 mm, 1.8 mm particle size, column was used at 25°C at a flow rate of 1.5 mL min -1 . UV detection was performed at 230 nm. The total time for chromatographic separation was 5.5 min with a total analysis time of 7.0 min. The method was validated for its linearity, precision, modal recovery and robustness.

show abstract

“…Minimum resolution and maximum retention times are set by the user and the program calculates the optimum by means of a search routine. Jacobsson et al [19] suggested a chromatographic response function (CRF) which modulates both separation quality and retention time for chiral separations. They also used neural network (NN) methods and compared them with MLR and PLS regression.…”

Section: Introductionmentioning

confidence: 99%

Liquid chromatography method development and optimization by statistical experimental design and chromatogram simulations

Harang

Josefson²

2001

Chromatographia

View full text Add to dashboard Cite

SummaryA liquid chromatographic method has been optimized by the use of an experimental design and chromatogram simulations. The strategy applied started with a statistical experimental design in which so-called beta coefficients were extracted from the mathematical model. Optimization was then performed by simulating the chromatographic separation with computer software.The effects of the variables (factors) are visualized in a way that is familiar to the analytical chemist. Simulation of chromatograms from combinations of factors within the experimental design is interactively available from a contour plot describing the minimum ~z (= k2/kJ of all possible combinations of peak pairs.Results from the optimization of an HPLC method, using the optimization strategy described above, are presented. Six peaks were separated from each otherwithin 11 min. The factors investigated were the amount of acetonitrile in the mobile phase, the concentration of phosphate buffer, and the concentration of octanesulfonate in the mobile phase.

show abstract

Optimisation of chromatographic separations by use of a chromatographic response function, empirical modelling and multivariate analysis

Cited by 27 publications

References 15 publications

Quantification of analytes in overlapping peaks from capillary electrophoresis using multivariate curve resolution‐alternating least squares methods

Quantification of analytes in overlapping peaks from capillary electrophoresis using multivariate curve resolution‐alternating least squares methods

Use of chemometrics for development and validation of an RP-HPLC method for simultaneous determination of haloperidol and related compounds

Liquid chromatography method development and optimization by statistical experimental design and chromatogram simulations

Contact Info

Product

Resources

About