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In-capillary derivatization and analysis of ephedrine and pseudoephedrine by micellar electrokinetic chromatography with laser-induced fluorescence detection.
J Chromatogr A. 2008 May 09; 1190(1-2):383-9.JC

Abstract

This paper describes an automatic rapid approach for in-capillary derivatization of ephedrine (E) and pseudoephedrine (PE) and subsequent sensitive determination of the derivatives by micellar electrokinetic chromatography (MEKC) with laser-induced fluorescence (LIF) detection using 4-fluoro-7-nitro-2,1,3-benzoxadiazole (NBD-F) as fluorescent reagent. The unique feature of this method is the capillary being used as a small reaction chamber, in which the sample, derivatization buffer and reagent solutions were injected directly into the capillary by tandem mode, followed by an electrokinetic step (5 kV, 15s) to enhance the mixing efficiency of analytes and reagent plugs. Standing a specified time of 1 min for reaction, the derivatives were then immediately separated and determined. Several parameters for in-capillary derivatization and subsequent MEKC separation were systematically investigated. Under these optimized conditions, a baseline separation of the two analytes was achieved within 10 min and the derivatization concentration limits of detection were found to be 4.8 ng mL(-1) for E and 1.6 ng mL(-1) for PE, respectively. The method was validated in terms of precision, linearity, accuracy and successfully applied for the determination of the two alkaloids in ephedra herb and its preparations.

Authors+Show Affiliations

Department of Chemistry, Lanzhou University, Lanzhou 730000, China.No affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article

Language

eng

PubMed ID

18374349

Citation

Zhou, Lei, et al. "In-capillary Derivatization and Analysis of Ephedrine and Pseudoephedrine By Micellar Electrokinetic Chromatography With Laser-induced Fluorescence Detection." Journal of Chromatography. A, vol. 1190, no. 1-2, 2008, pp. 383-9.
Zhou L, Zhou X, Luo Z, et al. In-capillary derivatization and analysis of ephedrine and pseudoephedrine by micellar electrokinetic chromatography with laser-induced fluorescence detection. J Chromatogr A. 2008;1190(1-2):383-9.
Zhou, L., Zhou, X., Luo, Z., Wang, W., Yan, N., & Hu, Z. (2008). In-capillary derivatization and analysis of ephedrine and pseudoephedrine by micellar electrokinetic chromatography with laser-induced fluorescence detection. Journal of Chromatography. A, 1190(1-2), 383-9. https://doi.org/10.1016/j.chroma.2008.03.024
Zhou L, et al. In-capillary Derivatization and Analysis of Ephedrine and Pseudoephedrine By Micellar Electrokinetic Chromatography With Laser-induced Fluorescence Detection. J Chromatogr A. 2008 May 9;1190(1-2):383-9. PubMed PMID: 18374349.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - In-capillary derivatization and analysis of ephedrine and pseudoephedrine by micellar electrokinetic chromatography with laser-induced fluorescence detection. AU - Zhou,Lei, AU - Zhou,Ximin, AU - Luo,Zhi, AU - Wang,Weiping, AU - Yan,Na, AU - Hu,Zhide, Y1 - 2008/03/14/ PY - 2008/01/05/received PY - 2008/02/29/revised PY - 2008/03/06/accepted PY - 2008/4/1/pubmed PY - 2008/8/14/medline PY - 2008/4/1/entrez SP - 383 EP - 9 JF - Journal of chromatography. A JO - J Chromatogr A VL - 1190 IS - 1-2 N2 - This paper describes an automatic rapid approach for in-capillary derivatization of ephedrine (E) and pseudoephedrine (PE) and subsequent sensitive determination of the derivatives by micellar electrokinetic chromatography (MEKC) with laser-induced fluorescence (LIF) detection using 4-fluoro-7-nitro-2,1,3-benzoxadiazole (NBD-F) as fluorescent reagent. The unique feature of this method is the capillary being used as a small reaction chamber, in which the sample, derivatization buffer and reagent solutions were injected directly into the capillary by tandem mode, followed by an electrokinetic step (5 kV, 15s) to enhance the mixing efficiency of analytes and reagent plugs. Standing a specified time of 1 min for reaction, the derivatives were then immediately separated and determined. Several parameters for in-capillary derivatization and subsequent MEKC separation were systematically investigated. Under these optimized conditions, a baseline separation of the two analytes was achieved within 10 min and the derivatization concentration limits of detection were found to be 4.8 ng mL(-1) for E and 1.6 ng mL(-1) for PE, respectively. The method was validated in terms of precision, linearity, accuracy and successfully applied for the determination of the two alkaloids in ephedra herb and its preparations. SN - 0021-9673 UR - https://www.unboundmedicine.com/medline/citation/18374349/In_capillary_derivatization_and_analysis_of_ephedrine_and_pseudoephedrine_by_micellar_electrokinetic_chromatography_with_laser_induced_fluorescence_detection_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0021-9673(08)00491-3 DB - PRIME DP - Unbound Medicine ER -