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Chemometric approach for development, optimization, and validation of different chromatographic methods for separation of opium alkaloids

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Abstract

The excessive and continuously growing interest in the simultaneous determination of poppy alkaloids imposes the development and optimization of convenient high-throughput methods for the assessment of the qualitative and quantitative profile of alkaloids in poppy straw. Systematic optimization of two chromatographic methods (gas chromatography (GC)/flame ionization detector (FID)/mass spectrometry (MS) and reversed-phase (RP)–high-performance liquid chromatography (HPLC)/diode array detector (DAD)) for the separation of alkaloids from Papaver somniferum L. (Papaveraceae) was carried out. The effects of various conditions on the predefined chromatographic descriptors were investigated using chemometrics. A full factorial linear design of experiments for determining the relationship between chromatographic conditions and the retention behavior of the analytes was used. Central composite circumscribed design was utilized for the final method optimization. By conducting the optimization of the methods in very rational manner, a great deal of excessive and unproductive laboratory research work was avoided. The developed chromatographic methods were validated and compared in line with the resolving power, sensitivity, accuracy, speed, cost, ecological aspects, and compatibility with the poppy straw extraction procedure. The separation of the opium alkaloids using the GC/FID/MS method was achieved within 10 min, avoiding any derivatization step. This method has a stronger resolving power, shorter analysis time, better cost/effectiveness factor than the RP-HPLC/DAD method and is in line with the “green trend” of the analysis. The RP-HPLC/DAD method on the other hand displayed better sensitivity for all tested alkaloids. The proposed methods provide both fast screening and an accurate content assessment of the six alkaloids in the poppy samples obtained from the selection program of Papaver strains.

 

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Abbreviations

CCCD:

Central composite circumscribed design

CD:

Codeine

DAD:

Diode array detector

DoE:

Design of experiments

DSC:

Differential scanning calorimetry

FID:

Flame ionization detector

FTIR:

Fourier transform infrared spectroscopy

GC:

Gas chromatography

HPLC:

High-performance liquid chromatography

ICH:

International conference on harmonization

MO:

Morphine

MS:

Mass spectrometry

NIST:

National institute of standardization and technology

NS:

Noscapine

OR:

Oripavine

RP:

Reverse-phase liquid chromatography

Rs:

Resolution

RSM:

Response Surface Methodology

PV:

Papaverine

TB:

Thebaine

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Acknowledgments

A part of this study was financially supported by ALKALOID A.D. Skopje.

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Authors and Affiliations

  1. Institute of Applied Chemistry and Pharmaceutical Analysis, Faculty of Pharmacy, University Ss. Cyril and Methodius, Vodnjanska 17, Skopje, 1000, Republic of Macedonia

    J. Acevska, R. Petkovska & A. Dimitrovska

  2. Institute of Pharmacognosy, Faculty of Pharmacy, University Ss. Cyril and Methodius, Vodnjanska 17, Skopje, 1000, Republic of Macedonia

    G. Stefkov & S. Kulevanova

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  1. J. Acevska
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  2. G. Stefkov
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  3. R. Petkovska
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  4. S. Kulevanova
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  5. A. Dimitrovska
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Correspondence to J. Acevska.

Additional information

Published in the special issue Euroanalysis XVI (The European Conference on Analytical Chemistry) with guest editor Slavica Ražić.

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Acevska, J., Stefkov, G., Petkovska, R. et al. Chemometric approach for development, optimization, and validation of different chromatographic methods for separation of opium alkaloids. Anal Bioanal Chem 403, 1117–1129 (2012). https://doi.org/10.1007/s00216-012-5716-1

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