气相色谱法测定6种不同基质化妆品中水杨酸甲酯含量

doi:10.3969/j.issn.1001-1803.2023.03.015

摘要/Abstract

摘要：

建立了气相色谱法（GC）测定6种基质化妆品中水杨酸甲酯的方法，并采用气相色谱-串联质谱法（GC-MS）对目标物进行定性确证。蜡基样品经乙酸乙酯-无水乙醇提取，其他基质样品经无水乙醇提取后，采用气相色谱-氢火焰离子化检测器进行测定。GC-MS采用全扫（SCAN）与选择离子监测（SIM）方式对结果进行确认。水杨酸甲酯质量浓度在5~500 mg/L范围内与其峰面积呈良好的线性关系（r=0.999 9）；6种基质在高、中、低三个浓度加标的平均回收率为96.9%~108.2%，相对标准偏差（RSD）均≤2.9%（n=6）；方法检出限为4 μg/g，定量限为100 μg/g；方法用于不同基质样品的分析，其中1批润唇膏检出水杨酸甲酯含量为0.083%，超出了欧盟对此类产品的限值要求。该方法快速、准确，适用于不同基质化妆品中水杨酸甲酯的定性定量分析，为化妆品中水杨酸甲酯的测定与筛查提供了技术支持。

关键词: 水杨酸甲酯, 气相色谱法, 气相色谱-串联质谱法, 化妆品

Abstract:

A method for the determination of methyl salicylate in 6 kinds of cosmetics bases by gas chromatography （GC） was established, and gas chromatography-mass spectrometry （GC-MS） was used to analyze for qualitative verification. The wax-based samples were extracted with ethyl acetate-absolute ethanol, and the other bases were extracted with anhydrous ethanol, and then were determined by GC equipped with hydrogen flame ionization detector （FID）. GC-MS adopt full SCAN and selective ion monitoring （SIM） methods to confirm the results. Linear relationship between the mass concentration of methyl salicylate and its peak area is kept in the range of 5-500 mg/L （r=0.999 9）, with the detection limit of 4 μg/g, and the quantification limit of 100 μg/g. The average recovery rate of the six bases spiked at high, medium and low concentrations are 96.9%-108.2%, and the RSDs （n=6） are all less than 2.9%. The method is used to analyze different commercially available samples. The content of methyl salicylate in one batch of the lip balm is 0.083%, which exceeds the maximum concentration recommended by Scientific Committee on Consumer Safety （SCCS）. The method is fast and accurate, suitable for the qualitative and quantitative analysis of methyl salicylate in different cosmetic bases, and provides technical support for the determination and screening of methyl salicylate in cosmetics.

Key words: methyl salicylate, gas chromatography, gas chromatography-tandem mass spectrometry, cosmetics

中图分类号:

TQ658

汪亚菁, 贾伯阳, 邬国庆, 邸铮. 气相色谱法测定6种不同基质化妆品中水杨酸甲酯含量[J]. 日用化学工业（中英文）, 2023, 53(3): 355-360.

Wang Yajing, Jia Boyang, Wu Guoqing, Di Zheng. Determination of methyl salicylate in 6 kinds of cosmetics bases by GC[J]. China Surfactant Detergent & Cosmetics, 2023, 53(3): 355-360.

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化妆品类型	最大使用量/%
水醇基香水	0.600
非驻留类皮肤和发用产品（洗手产品除外）	0.060
洗手产品	0.600
驻留类皮肤和发用产品（非气雾剂）	0.060
面部彩妆产品	0.050
口红和润唇膏	0.030
眼部彩妆产品和卸妆液	0.002
牙膏	2.520
漱口水（6~10岁）	0.100
漱口水（10岁以上）	0.600
口腔喷雾剂	0.650
脱毛类喷雾剂/气雾剂	0.003
头发产品（喷雾剂/气雾剂）	0.009
身体乳喷雾	0.040

样品	加标量/ μg	测定值/ μg	回收率/ %	平均回收率/%	RSD/ %	样品	加标量/ μg	测定值/ μg	回收率/ %	平均回收率/%	RSD/ %
爽肤水	50.05	44.25	88.2	96.9	1.2	护肤橄榄油	50.05	47.25	94.7	95.2	1.4
	250.2	241.5	96.2		1.0		250.2	244.6	97.6		0.6
	2 502	2 644	106.1		1.3		2 502	2 335	93.4		0.8
W/O型乳液	50.05	49.02	97.8	100.6	0.9	粉饼	50.05	51.73	103.8	106.0	2.9
	250.2	253.6	101.3		0.6		250.2	267.7	107.1		1.4
	2 502	2 569	102.7		0.6		2 502	2 688	107.2		2.0
O/W型乳霜	50.05	47.65	95.6	98.4	1.5	润唇膏	50.05	51.80	103.3	108.2	1.0
	250.2	246.6	98.3		2.3		250.2	274.7	109.3		1.3
	2 502	2 546	101.3		1.8		2 502	2 813	112.1		2.0