液相色谱-串联质谱法快速测定化妆品中游离的乙醇胺类物质

doi:10.3969/j.issn.2097-2806.2024.05.016

Abstract

Abstract:

A stable isotope dilution-liquid chromatography-tandem mass spectrometry method was established for the determination of three free ethanolamine compounds in cosmetics. The ethanolamine compounds were extracted with isopropanol and separated by Kinetex HILIC chromatographic column with isocratic elution using acetonitrile and 0.1% formic acid-water solution （V/V）. The samples were ionized by positive ion mode of electrospray ionization source and determined by multiple reaction monitoring （MRM） mode. Optimization was conducted using single factor experiments for the best conditions of determination. The optimum determination conditions are using isopropanol by ultrasonic extraction for 20 min. Under this combination of conditions, the ranges of internal standard curves for monoethanolamine, diethanolamine, and triethanolamine are 5.0-200 μg/L, 2.0-200 μg/L and 1.0-200 μg/L, respectively, with the correlation coefficient R² greater than 0.999. The average recovery rate ranges from 87.1% to 97.0%, and relative standard deviations （RSDs） are between 1.68%-6.57%. The limit of detection and limit of quantification are 3.00-15.0 µg/kg and 10.0-50.0 µg/kg, respectively. The established method is used for the detection of 61 cosmetic samples. The method is simple operation, accurate quantification, stable recovery, high sensitivity and high precision and suitable for the determination of free ethanolamine compounds in cosmetics.

Key words: liquid chromatography-tandem mass spectrometry, rapid determination, cosmetics, ethanolamine compounds

CLC Number:

TQ658

Guangfeng Zeng, Zhiyuan Wang, Jianjun Xie, Lu Wang, Yingye Hou, Jie Dong. Rapid determination of free ethanolamine compounds in cosmetics by liquid chromatography-tandem mass spectrometry[J].China Surfactant Detergent & Cosmetics, 2024, 54(5): 614-620.

Figures/Tables 9

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References 19

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化合物	母离子（m/z）	子离子（m/z）	去簇电压/V	碰撞能量/eV
一乙醇胺	62.1	44.1^*	45.2	16.0
一乙醇胺	62.1	45.1	45.2	20.0
二乙醇胺	106.0	70.0	50.0	22.0
二乙醇胺	106.0	88.0^*	54.1	16.0
三乙醇胺	150.0	132.0^*	55.1	18.2
三乙醇胺	150.0	88.0	55.1	24.2
一乙醇胺-D7	66.1	48.1^*	47.9	13.9
二乙醇胺-D4	110.0	92.1^*	48.0	18.0
三乙醇胺-D15	162.2	144.2^*	65.5	21.8

化合物	基质效应/%
化合物	精油	唇膏	面霜
一乙醇胺	-55.2	-26.3	-23.7
二乙醇胺	-59.3	-47.2	-49.4
三乙醇胺	-40.1	-38.7	-39.4

化合物	线性方程	R²	LOD/（μg/kg）	LOQ/（μg/kg）
三乙醇胺	y=0.007 42x-0.004 25	0.999 7	3.00	10.0
二乙醇胺	y=0.001 07x+0.078 5	0.999 5	5.00	20.0
一乙醇胺	y=0.013 0x+0.006 32	0.999 6	15.0	50.0

基质	化合物	加标量/（μg/kg）	实测值/（μg/kg）	平均回收率/%	RSD/%
精油	三乙醇胺	10.0，20.0，50.0	9.15，18.9，48.1	91.5，94.5，96.2	4.05，2.64，3.74
	二乙醇胺	20.0，40.0，100	17.6，37.0，95.8	88.0，92.5，95.8	3.90，3.51，2.40
	一乙醇胺	50.0，100，250	45.1，91.6，234	90.2，91.6，93.6	4.13，4.05，2.77
唇膏	三乙醇胺	10.0，20.0，50.0	8.71，19.1，47.7	87.1，95.5，95.4	6.57，2.78，2.85
	二乙醇胺	20.0，40.0，100	18.1，38.2，94.2	90.5，95.5，94.2	5.13，2.15，3.73
	一乙醇胺	50.0，100，250	45.8，96.6，241	91.6，96.6，96.4	3.10，1.75，4.80
面霜	三乙醇胺	10.0，20.0，50.0	9.48，19.4，48.4	94.8，97.0，96.8	2.77，1.68，3.33
	二乙醇胺	20.0，40.0，100	18.0，38.2，96.1	90.0，95.5，96.1	3.57，2.28，3.77
	一乙醇胺	50.0，100，250	43.8，94.1，242	87.6，94.1，96.8	4.66，2.41，4.15

Rapid determination of free ethanolamine compounds in cosmetics by liquid chromatography-tandem mass spectrometry

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