Microdialysis of salicylic acid from viscous emulsion samples prior to high-performance liquid chromatographic determination

doi:10.1016/S0021-9673(01)00562-3

Journal of Chromatography A

Volume 912, Issue 1, 30 March 2001, Pages 39-43

https://doi.org/10.1016/S0021-9673(01)00562-3 Get rights and content

Abstract

A micro-dialysis method was developed to isolate aqueous salicylic acid from viscous emulsion samples prior to HPLC determination. The optimal conditions for obtaining dialysis efficiency of salicylic acid as well as chromatographic conditions were investigated. Experimental results indicated that the dialysis achieved at pH 2.0 (0.025 M phosphate solution), 0.5 M NaCl addition, and 50-μl/min flow-rate of perfusion stream offered an optimal result. The proposed method provided a simple procedure for isolating salicylic acid from viscous emulsion samples. Application was illustrated by the analysis of salicylic acid in cosmetic products.

Introduction

Liquid–liquid extraction is a conventional pre-treatment step in the determination of interested species in samples. However, it usually is time-consuming and requires a large quantity of organic solvents, which is a potential health risk and may cause environmental pollution. Besides, in the extraction of viscous/emulsion samples, the unclear interfacial layer often influences the separation efficiency.

For complicated matrix samples, membrane-based separations have been applied as useful tools for sample pretreatment or sampling [1]. Thus, on-line dialysis has been widely used in on-line bioprocess monitoring [2], [3], [4], [5]. A commercial Gilson ASTED system on-line combined with an HPLC instrument was thus developed and widely used. In order to increase the membrane area available for diffusion, hollow-fiber membranes was used instead of planar ones. Recently, micro-dialysis has been extensively applied in biotechnological and biomedical research [6], [7], [8], [9]. Compared to the conventional extraction protocol, micro-dialysis separation has the advantages of easy operation, rapid isolation of interest components from turbid and complicate matrix samples, and free or less-use organic solvents. From the application of on-line dialysis in the sampling of bovine serum, muscle tissue, plasma, and for pharmacokinetic studies [6], [7], [8], [9], [10], [11], [12], [13], [14], dialysis has the potential to be the alternative to conventional separation techniques for non-biological samples. However, except for the on-line dialysis system used for the analysis of liquid food samples [15], [16], [17], [18], [19], micro-dialysis has seldom been approached in consumer products with a complex matrix.

Salicylic acid is used as preservative of food products, paste, glue, and hides. Recently, it has been widely used as a whitening agent in cosmetic products. In these viscous emulsion samples, it is difficult to use conventional separation techniques, such as liquid–liquid extraction, solid-phase extraction, and solid-phase micro-extraction, to achieve the isolation. In this paper, with the described advantages, the micro-dialysis technique is systematically investigated in order to develop a simple pretreatment process for viscous/emulsion samples prior to HPLC determination.

Section snippets

Apparatus

The HPLC used in this work was a Shimadzu LC-9A system (Shimadzu, Kyoto, Japan), and a Waters 484 tunable absorbance detector (Waters, Milford, MA, USA) with a 20-μl flow cell. The detection wavelength was set at 230 nm. A reversed-phase C₁₈ column (25 cm×4.6 mm I.D. 5-μm particle size) (Supelco, Bellefonte, PA, USA) was used for separation. A Rheodyne 7125 injector (Cotati, CA, USA) with a 20-μl external loop was used for sample introduction. A Chromatocorder 12 Integrator (SIC, Tokyo, Japan)

Results and discussions

In order to verify the applicability of the proposed micro-dialysis isolation method, factors that affect the dialysis efficiency such as the flow-rate of perfusion, the pH and salt addition in sample solution, as well as the chromatographic conditions were studied thoroughly to optimize the sampling and analytical conditions.

Conclusion

This paper investigated the potential of micro-dialysis applied in the isolation of salicylic acid from viscous/emulsion samples such as cosmetics. The results indicate that the proposed micro-dialysis can be an alternative to conventional extraction step prior to HPLC determination with the advantages of easy operation, less time-expense, and free-use organic solvent.

Acknowledgments

The authors thank the National Science Council of the ROC for financial support under the grant number NSC-88-2113-M-005-002.

References (24)

N.C. van de Merbel
J. Chromatogr. A
(1999)
N.C. van de Merbel et al.
Anal. Chim. Acta
(1995)
N.C. van de Merbel et al.
J. Chromatogr. A
(1996)
N.C. van de Merbel
Trends Anal. Chem.
(1997)
N. Torto et al.
Trends Anal. Chem.
(1999)
G. Shi et al.
Anal. Chim. Acta
(1999)
T.H. Tsai et al.
Intl. J. Pharm.
(1999)
F.C. Cheng et al.
J. Chromatogr. B
(1999)
T.H. Tsai et al.
J. Chromatogr. B
(1999)
F. Sadeghipour et al.
J. Pharm. Biomed. Anal.
(1998)

K. Johansen et al.

J. Chromatogr. B

(1997)

R.J. Slingerland et al.

J. Chromatogr. B

(1998)

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A new approach to determine salicylic acid in human urine and blood plasma based on negative electrospray ion mobility spectrometry after selective separation using a molecular imprinted polymer
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Therefore, doping control laboratories have to establish a quantitative and qualitative method for the analysis of this drug in various biological matrixes. For the determination of salicylic acid in different samples, a number of analytical methodologies have been reported, including high performance liquid chromatography (HPLC) with various detection systems [2,5–7], capillary electrophoresis [8], liquid chromatography/quadruple-time of flight mass spectrometry (LC–QTOF–MS) [4,9], gas chromatography/mass spectrometry (GC–MS) [3,10,11] and a variety of electrochemical methods [12,13]. Usually, these standard methods have a good selectivity due to using a powerful separation techniques (e.g., GC, LC, …).
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Microdialysis of salicylic acid from viscous emulsion samples prior to high-performance liquid chromatographic determination

Abstract

Introduction

Section snippets

Apparatus

Results and discussions

Conclusion

Acknowledgments

J. Chromatogr. A

Anal. Chim. Acta

J. Chromatogr. A

Trends Anal. Chem.

Trends Anal. Chem.

Anal. Chim. Acta

Intl. J. Pharm.

J. Chromatogr. B

J. Chromatogr. B

J. Pharm. Biomed. Anal.

J. Chromatogr. B

J. Chromatogr. B