气相色谱-质谱/质谱法测定美白化妆品中5种酚类物质

doi:10.3969/j.issn.1001-1803.2022.01.013

Abstract

Abstract:

A method based on gas chromatography-tandem mass spectrometry （GC-MS/MS） was developed for the analysis of 5 phenolics compounds （phenol, hydroquineone, resorcinol, 4-butylresorciol, phenylethyl resorciol） in cosmetics. The phenolics compounds were extracted from cosmetics by supersonic extraction with 0.03 mol/L potassium dihydrogen phosphate solution, purified by HLB solid phase extraction column, and analyzed via GC-MS/MS after filtration with organic filtration membrane （0.22 μm）. Separation was performed on a SH-Rtx-1701MS chromatographic column （30 m×0.25 mm×0.25 μm） by GC-MS/MS with an electrospray ionization （EI） source in the MRM mode. The external standard method was used for quantitative determination. The 5 phenolics compounds can be analyzed within 10 min under the optimum conditions, and it exhibits a good linearity with the standard correlation coefficients （R²） of not less than 0.999 in their respective concentration ranges of 5-200 μg/L. The limited of determination （LODs） are 1.5-3.0 μg/L and the limits of quantitation （LOQs） are 5.0-10.0 μg/L, respectively. The recoveries at three standards are 73.5%-111.8%, and the relative standard deviations （RSDs） are between 1.0% and 11.1% （n=6）. The proposed method is accurate, reliable, simple and convenient, and is suitable for determination of phenol whitening active components in cosmetics.

Key words: gas chromatography tandem mass spectrometry （GC-MS/MS）, solid phase extractions, cosmetics, phenolic compounds （phenols）

CLC Number:

TQ658

Xiao Zhaojing,Tong Lanyan,Li Genrong,Dai Zhenghua,Zhou Zhaoxu,Yu Wenqin. Determination of five phenolics compounds in whitening cosmetics by gas chromatography-tandem mass spectrometry[J].China Surfactant Detergent & Cosmetics, 2022, 52(1): 84-90.

Figures/Tables 9

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References 22

[1]	Yang Yanwei, Zhu Ying. Progress on effect and determination of skin whitening anti freckle components in cosmetics[J]. Journal of Environment and Health, 2010, 27(8) : 745-748.
[2]	Zhou Xiao, Tang Jiali, Gong Yingkun. Research progress in detection methods of whitening active components in cosmetics[J]. Applied Chemical Industry, 2020, 49(1) : 244-247.
[3]	Li Qing, Xie Xiaoping, Gu Meifang. Hygienic toxicological test results of 229 whitening and freckle removing cosmetics[J]. South China Journal of Preventive Medicine, 2006, 32, (5) : 76-77.
[4]	Cui Xia, Zou Mingqiang, Hu Xiuli, et al. Research progress on potential toxicity of hydroquinone in skin whitening agents[J]. Chinese Journal of Public Health, 2008, 24(7) : 873-874.
[5]	Chen Peijin, Liang Hong, Xiao Feng, et al. Simultaneous determination of 10 whitening and 2 prohibited components in cosmetics by high performance liquid chromatography[J]. Journal of Instrumental Analysis, 2017, 36(3) : 403-408.
[6]	Li Li, Yang Run. Determination of content of phenylethyl resorcinol in whitening and freckle-removing cosmetics by HPLC[J]. Jiangsu Journal of Preventive Medicine, 2014, 25(5) : 13-14.
[7]	Gao Jiamin, Dai Jing, Li Hongxia, et al. Simultaneous determination of seventeen kinds of whitening ingredients in cosmetics by high performance liquid chromatography[J]. Chinese Journal of Pharmaceutical Analysis, 2019, 39(9) : 1643-1650.
[8]	Zhao Jiangli, Zhang Ming, Zhang Xiru, et al. Improvement on determination of hydroquinone and phenol in whitening cosmetics by HPLC[J]. Chinese Journal of Pharmaceutical Analysis, 2017, 37(3) : 508-513.
[9]	Wu Chusen, Wang Bin, Liang Ming, et al. Determination of 4 banned phenols in cosmetics by high performance liquid chromatography[J]. Journal of Instrumental Analysis, 2019, 38(8) : 985-989.
[10]	Jiang Sheng, Wang Ming, Yang Xiaoshan, et al. Determination of phenol and hydroquinone in cosmetics by capillary column gas chromatography[J]. Application of Science and Technology, 2016 (1) : 34-34.
[11]	Yang Jingzhi, Sun Yanhua, Zhou Jie, et al. Determination of trace phenol by KBrO₃-KBr UV spectrophotometry[J]. Analytical Laboratory, 1999, 18(4) : 57-59.
[12]	Zhang Qianli, Liu Xiaoyan, Wang Xiuling. A study of the determination of the preservative phenol by UV spectrophotometry[J]. Journal of University of Science and Technology of Suzhou (Natural Science), 2017, 24(4) : 53-56.
[13]	Han Kang, Zhai Xueliang. Determination of hydroquinone, phenol and preservatives in cosmetics by capillary electrophoresis[J]. Chinese Journal of Analysis Laboratory, 2011, 30(1) : 107-109.
[14]	Liu Yingchun, Ji Huagui, Chen Jie, et al. Simultaneous determination of 7 phenolics compounds in cosmetics by capillary column-GC[J]. China Journal Health Laboratory Technology, 2015, 25(20) : 3448-3450.
[15]	Liang Ying, Xu Wenjia, Fu Ceyi, et al. Determination of four kinds of whitening efficacy ingredients in cosmetics by high performance chromatography tandem mass spectrometry[J]. Journal of Environment and Health, 2019, 36(1) : 53-56.
[16]	Chen Shaobo, Pu Yunyue, Yu Wenjing, et al. Determination of phenol and hydroquinone in cosmetics by gas chromatography mass spectrometry[J]. Analysis and Testing Technology and Instruments, 2017, 23(3) : 176-179.
[17]	Zhai Yu, Shang Boyang, Huang Qing, et al. Determination of phenol and hydroquinone in whitening and freckle-removing cosmetics by GC-MS[J]. Journal of Ningxia Medical University, 2019, 41(1) : 40-43.
[18]	Wu Yongliang, Li Yanyuan, Peng Yuntie. Determination of seven phenolic compounds in mainstream cigarette smoke by gas chromatography tandem mass spectrometry[J]. Journal of Chinese mass Spectrometry Society, 2018, 39(3) : 376-384.
[19]	Dou Yue, Tian Jinqiang, Wang Qianlei, et al. Determination of five fluorescent whitening agents in cosmetics by high performance liquid chromatography-tandem mass spectrometry[J]. China Surfactant Detergent & Cosmetics, 2020, 5(6) : 427-432.
[20]	Wang Guanying. Simultaneous determination of 6 kinds of phenols in cosmetics by gas chromatography tandem mass spectrometry[J]. China Cleaning Industry, 2016, 8:73-77.
[21]	General Administration of Quality Supervision. Determination of 10 whitening and freckl-removing components in cosmetics high performance liquid chromatography. GB/T 35954-2018[S]. Beijing: China Standard Press, 2018.
[22]	Lei Xiang, Lei Chen, Mo Cehui, Determination of trace perfluoroalkyl carboxylic acids in edible crop matrices: matrix effect and method development[J]. Journal of Agricultural and Food Chemistry, 2017, 65(39) : 8763-8772. doi: 10.1021/acs.jafc.7b02677 pmid: 28905619

序号	化合物	保留时间/min	母离子（m/z）	子离子（m/z）	碰撞能量/eV
1	苯酚	3.984	94.0	66.1^*,55.0	16/18
2	氢醌	5.977	110.0	81.1^*,53.1	18/26
3	间苯二酚	6.095	110.0	82.1^*,53.1	12/28
4	4-丁基间苯二酚	7.163	166.0	123^*,67.1,95.1	10/12
5	苯乙基间苯二酚	9.031	214.0	199^*,152,91.1	8/24

化合物	回收率/%
化合物	HLB	WAX	MAX
苯酚	104.2	102.8	51.5
氢醌	109.6	74.8	57.9
间苯二酚	115.2	124.2	63.5
4-丁基间苯二酚	111.8	90.6	44.3
苯乙基间苯二酚	104.9	80.3	10.3

化合物	线性范围/（μg/L）	线性方程	相关系数	检出限/（μg/L）	定量限/（μg/L）
苯酚	5~200	Y=7.26×10⁴X+2.20×10⁴	0.999 4	1.5	5.0
氢醌	5~200	Y=7.44×10³X-1.67×10⁴	0.999 8	3.0	10.0
间苯二酚	5~200	Y=1.84×10⁴X-4.53×10⁵	0.999 4	1.5	5.0
4-丁基间苯二酚	5~200	Y=1.65×10⁴X-4.44×10⁴	0.999 7	1.5	5.0
苯乙基间苯二酚	5~200	Y=1.79×10⁴X-1.02×10⁵	0.999 6	1.5	5.0

化合物	加标浓度/（μg/L）	水剂		乳液		霜膏		粉剂
化合物	加标浓度/（μg/L）	回收率/%	精密度/%	回收率/%	精密度/%	回收率/%	精密度/%	回收率/%	精密度/%
苯酚	10.0	85.6	3.8	73.5	1.9	74.4	2.0	74.4	2.0
	50.0	96.9	4.3	89.6	2.6	88.3	1.4	88.3	1.7
	100.0	101.2	2.5	104.6	8.0	103.3	8.6	103.3	8.6
氢醌	10.0	83.3	9.3	88.6	9.7	73.5	6.3	73.5	3.1
	50.0	96.3	8.4	101	3.9	93.4	8.0	77.9	11.1
	100.0	95.2	2.9	108.5	10.6	97.4	4.3	97.4	4.3
间苯二酚	10.0	101	4.9	89.3	2.9	74.6	2.7	74.6	2.7
	50.0	95.7	1.5	102.2	1.4	82.2	6.3	82.2	6.3
	100.0	103.9	0.3	102	5.6	87.2	1.2	96.9	1.3
4-丁基间苯二酚	10.0	88.8	3.4	89.4	2.1	76.1	1.5	76.1	1.5
	50.0	111.1	1.6	107.2	3.5	83.4	2.8	83.4	2.8
	100.0	99.9	1.0	111.8	7.5	97.2	6.8	97.2	6.8
苯乙基间苯二酚	10.0	81.5	10.2	99.1	7.3	85.1	2.8	85.1	9.0
	50.0	92.4	6.1	101.3	10.9	85	3.5	85	3.5
	100.0	109.9	9.8	103.6	9.0	97.7	10.6	103.5	10.6

Determination of five phenolics compounds in whitening cosmetics by gas chromatography-tandem mass spectrometry

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