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

摘要/Abstract

摘要：

建立稳定同位素稀释-液相色谱-串联质谱法（LC-MS/MS）测定化妆品中游离的3种乙醇胺类物质。样品经异丙醇提取后，使用乙腈和0.1%甲酸-水溶液（体积分数，下同）梯度洗脱，Kinetex HILIC色谱柱分离，电喷雾电离源正离子模式电离，多反应监测模式进行测定。采用单因素试验优化得到最佳前处理条件：提取溶剂为异丙醇、超声波提取、提取时间为20 min、不改变样品pH直接提取。使用内标法曲线定量，一乙醇胺、二乙醇胺和三乙醇胺内标曲线分别在5.0~200，2.0~200和1.0~200 μg/L范围内线性关系良好，相关系数R²大于0.999，平均回收率范围在87.1%~97.0%，相对标准偏差（RSDs）在1.68%~6.57%之间，方法检出限为3.00~15.0 µg/kg，定量限为10.0~50.0 µg/kg。建立的方法适用于61批次化妆品样品的检测。该方法操作简便，定量准确，回收率稳定、灵敏度高、精密度高，适用于测定化妆品中的乙醇胺类物质。

关键词: 液相色谱-串联质谱法, 快速测定, 化妆品, 乙醇胺

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

中图分类号:

TQ658

曾广丰, 王志元, 谢建军, 王璐, 侯颖烨, 董洁. 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[J]. 日用化学工业（中英文）, 2024, 54(5): 614-620.

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.

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参考文献 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