Rapid analysis of melamine in infant formula by sweeping-micellar electrokinetic chromatography

I. L. Tsai, Shao W. Sun, Hsiao W. Liao, Shu Chiao Lin, Ching H. Kuo

Research output: Contribution to journalArticle

66 Citations (Scopus)

Abstract

In the present study, an analytical method using capillary electrophoresis with on-line preconcentration technique was developed for rapid determination of melamine in infant formula. Both stacking and sweeping preconcentration techniques had been investigated for the comparison of their effectiveness in melamine analysis. The limit of detection of melamine standard was 0.5 ng/mL for the field amplified sample stacking (FASS) technique and 9.2 ng/mL for the sweeping technique. Although the FASS technique provided better concentration efficacy than the sweeping technique, the matrix effect was more profound with the former. Matrix effect was evaluated by comparing the enhancement factor (EF) of melamine standard and post-extraction spiked infant formula solution. The EF was changed from 429.86 ± 9.81 to the level less than 133.31 with significant peak distortion in the FASS system, and it was remained unchanged in the sweeping system. Sweeping-micellar electrokinetic chromatography (sweeping-MEKC) was demonstrated to be most suitable for real sample analysis. Under optimum sweeping-MEKC conditions, melamine content in infant formulas could be determined within 6 min. The developed solid phase extraction (SPE) procedures coupled with the sweeping-MEKC method was subjected to method validation. Run-to-run repeatability (n = 3) and day-to-day reproducibility (n = 3) of peak area were within 3.6% and 4.8% RSD, respectively. The accuracy was tested by spiking 0.5 and 2 μg/mL of melamine standard in the melamine contaminated milk powder provided by the European Commission, and the recoveries were 93.4 ± 0.5% and 98.7 ± 0.4%, respectively. Results of this study show a great potential for the sweeping-MEKC method as a tool for the fast screening of melamine in infant formulas.

Original languageEnglish
Pages (from-to)8296-8303
Number of pages8
JournalJournal of Chromatography A
Volume1216
Issue number47
DOIs
Publication statusPublished - Nov 20 2009
Externally publishedYes

Fingerprint

Infant Formula
Chromatography
Capillary electrophoresis
melamine
Solid Phase Extraction
Capillary Electrophoresis
Powders
Limit of Detection
Screening
Milk
Recovery

Keywords

  • Infant formula
  • Melamine
  • Stacking
  • Sweeping

ASJC Scopus subject areas

  • Biochemistry
  • Analytical Chemistry
  • Organic Chemistry

Cite this

Rapid analysis of melamine in infant formula by sweeping-micellar electrokinetic chromatography. / Tsai, I. L.; Sun, Shao W.; Liao, Hsiao W.; Lin, Shu Chiao; Kuo, Ching H.

In: Journal of Chromatography A, Vol. 1216, No. 47, 20.11.2009, p. 8296-8303.

Research output: Contribution to journalArticle

Tsai, I. L. ; Sun, Shao W. ; Liao, Hsiao W. ; Lin, Shu Chiao ; Kuo, Ching H. / Rapid analysis of melamine in infant formula by sweeping-micellar electrokinetic chromatography. In: Journal of Chromatography A. 2009 ; Vol. 1216, No. 47. pp. 8296-8303.
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AB - In the present study, an analytical method using capillary electrophoresis with on-line preconcentration technique was developed for rapid determination of melamine in infant formula. Both stacking and sweeping preconcentration techniques had been investigated for the comparison of their effectiveness in melamine analysis. The limit of detection of melamine standard was 0.5 ng/mL for the field amplified sample stacking (FASS) technique and 9.2 ng/mL for the sweeping technique. Although the FASS technique provided better concentration efficacy than the sweeping technique, the matrix effect was more profound with the former. Matrix effect was evaluated by comparing the enhancement factor (EF) of melamine standard and post-extraction spiked infant formula solution. The EF was changed from 429.86 ± 9.81 to the level less than 133.31 with significant peak distortion in the FASS system, and it was remained unchanged in the sweeping system. Sweeping-micellar electrokinetic chromatography (sweeping-MEKC) was demonstrated to be most suitable for real sample analysis. Under optimum sweeping-MEKC conditions, melamine content in infant formulas could be determined within 6 min. The developed solid phase extraction (SPE) procedures coupled with the sweeping-MEKC method was subjected to method validation. Run-to-run repeatability (n = 3) and day-to-day reproducibility (n = 3) of peak area were within 3.6% and 4.8% RSD, respectively. The accuracy was tested by spiking 0.5 and 2 μg/mL of melamine standard in the melamine contaminated milk powder provided by the European Commission, and the recoveries were 93.4 ± 0.5% and 98.7 ± 0.4%, respectively. Results of this study show a great potential for the sweeping-MEKC method as a tool for the fast screening of melamine in infant formulas.

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