Determination of tranexamic acid in essential cosmetics by pre-column derivatization capillary electrophoresis coupled with electrogenerated chemiluminescence detection

doi:10.3724/SP.J.1123.2019.12002

Abstract

Abstract:

N-Methylation of tranexamic acid yields an unique derivative, which generates strong co-luminescence signals in the presence of an electrochemiluminescence reagent such as Ru(bpy)₃²⁺. Using this principle, we established a highly selective analytical method based on pre-column derivatization capillary electrophoresis coupled with electrogenerated chemiluminescence detection for determining the tranexamic acid content in essential cosmetics. The addition of a ternary ionic association gel, Mg²⁺-trehalose-SiO₃^2-, in the components of background electrolyte greatly improved the electrophoretic separation efficiency. Under the optimized assay conditions, two electrophoretic peaks attributed to the derivatives of tranexamic acid and its internal standard (sarcosine) were completely separated in 500 s, and their electrophoretic peak intensities ratio showed a good linear relationship with the initial concentration of tranexamic acid in the range of 10-750 μmol/L (correlation coefficient r²=0.9993). The limit of detection was estimated to be 3.6 μmol/L (S/N=3). Moreover, the internal standard method was further applied to the quantitative determination of tranexamic acid content in three kinds of toothpaste and two kinds of nutrient solutions in facial masks. The results showed that the average tranexamic acid content in three toothpaste samples was 4.05, 0.24, and 6.06 mg/g, while that in two facial masks was 51.3 and 7.98 mg/mL. The recoveries for the above-mentioned samples were within the range 92.5% to 104.0%, implying satisfactory results.

Key words: capillary electrophoresis (CE), electrogenerated chemiluminescence (ECL), pre-column derivatization, tranexamic acid (TA), electrophoretic separation additive

WANG Rong, ZHOU Min, WANG Suxia, LIAO Yuan, FAN Xue, MA Yongjun. Determination of tranexamic acid in essential cosmetics by pre-column derivatization capillary electrophoresis coupled with electrogenerated chemiluminescence detection[J]. Chinese Journal of Chromatography, 2020, 38(8): 968-974.

Figures/Tables 5

Fig. 1 Contrastive electropherograms of the mixed standard solution of tranexamic acid (TA) and sarcosine (Sar) (a) before and (b) after the derivatization reaction 1. unknown derivative form formaldehyde reagent; 2. TA derivative; 3. Sar derivative. TA: 100 μmol/L; Sar: 25.0 μmol/L.

Fig. 2 Effect of the added amount of Mg2+-trehalose-SiO32- (MTS-gel) on the electrophoresis resolution between TA and Sar derivatives Δt: difference of the migration time of Sar and TA.

Fig. 3 RRS spectra of MTS-gel with the different substance constituent ratio (R) of SiO32- to Mg2+ A set of curves (a-f) shows influence of the MTS-gel concentrations on their RRS peak intensities when fixing a constant R value (R=6). Inset shows the variation of the slope (k) of linear fitting equations existed between RRS peak intensities of MTS-gel and its concentrations when modifying the R value (R=0-10). MTS-gel: a. 200 μmol/L; b. 250 μmol/L: c. 300 μmol/L; d. 350 μmol/L: e. 400 μmol/L; f. 450 μmol/L.

Fig. 4 Serial electrophoregrams of the standard solution samples with different TA concentrations for determination by internal standard method Sar: 25.0 μmol/L. TA: a. 25.0 μmol/L; b. 50.0 μmol/L; c. 100 μmol/L; d. 250 μmol/L; e. 500 μmol/L.

Table 1 Determination results of tranexamic acid content in real samples (n=3)

Sample	Found value/(mg/g) (mean±S. D.)	Spiked TA/(mg/g)	Total found value/(mg/g) (mean±S. D.)	Mean recovery/%
S. D.: standard deviation. * This unit of measurement is of mg/mL.
Toothpaste 1^#	4.05±0.14	0.80	4.80±0.13	93.8
Toothpaste 2^#	0.24±0.01	0.40	0.61±0.03	92.5
Toothpaste 3^#	6.06±0.09	2.00	7.93±0.20	93.5
Facial mask 1^#	51.3±0.1^*	40.0^*	92.1±0.3^*	102.0
Facial mask 2^#	7.98±0.15^*	3.00^*	11.1±0.4^*	104.0

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