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

Abstract

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

CLC Number:

TQ658

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.

Figures/Tables 6

Fig. 1

Tab. 1

Fig. 2

Tab. 2

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Fig. 4

References 20

[1]	European Chemicals AgencyECHA. Methyl salicylate[EB/OL]. (2021-11-24) [2022-03-24]. https://echa.europa.eu/substance-information/-/substanceinfo/100.003.925.
[2]	Fiume M Z, Coordinator M, Andersen F A. Safety assessment of salicylic acid, butyloctyl salicylate, calcium salicylate, C12-15 alkyl salicylate, capryloyl salicylic acid, hexyldodecyl salicylate, isocetyl salicylate, isodecyl salicylate, magnesium salicylate, mea-salicylate, ethylhexyl salicylate,potassium salicylate, methyl salicylate, myristyl salicylate, sodium salicylate, tea-salicylate, andtridecyl salicylate[J]. International Journal of Toxicology, 2003, 22 (3) : 1-108. doi: 10.1177/1091581803022S203
[3]	Cosmetic Ingredient ReviewCIR. Amended Safety Assessment of Salicylic Acid and Salicylates as Used in Cosmetics[EB/OL]. (2019-09-04) [2022-03-24]. https://online.personalcarecouncil.org/ctfa-static/online/lists/cir-pdfs/FR766.pdf.
[4]	Health Canada. Draft screening assessment-Salicylates group[EB/OL]. (2020-03-13) [2022-03-24]. https://www.canada.ca/en/environment-climate-change/services/evaluating-existing-substances/draft-screening-assessment-salicylates-group.html.
[5]	National Medical Products Administration. Announcement of the National Medical Products Administration on Issuing the “Catalogue of Used Cosmetic Raw Materials (2021 Edition)” (2021 No. 62)[EB/OL]. (2021-04-27) [2022-03-24]. https://www.nmpa.gov.cn/zhuanti/hzhpxch2021/hzhp2021fgwj/20210430162707173.html.
[6]	National Medical Products Administration. Announcement of the National Medical Products Administration on the Release of Safety and Technical standards for Cosmetics (2015 Edition) (2015 No. 268) [EB/OL]. (2015-12-23) [2022-03-24]. https://www.nmpa.gov.cn/hzhp/hzhpggtg/hzhpqtgg/20151223120001986.html.
[7]	European Union. Regulation (EC) No 1223/2009 [EB/OL]. (2022-03-01) [2022-03-24]. https://eur-lex.europa.eu/eli/reg/2009/1223.
[8]	European Chemicals Agency ECHA. Committee for Risk Assessment (RAC) Opinion proposing harmonised classification and labelling at EU level of Methyl salicylate[EB/OL]. (2019-09-20) [2022-03-24]. https://echa.europa.eu/documents/10162/ea33d742-d73f-a7a7-8bca-be3679b713e0.
[9]	Scientific Committee on Consumer SafetySCCS. OPINION on Methyl salicylate[EB/OL]. (2021-10-27) [2022-03-24]. https://ec.europa.eu/health/system/files/2021-11/sccs_o_255_0.pdf.
[10]	Ministry of Health of the People’s Republic of China. National Food Safety Standard Food Additives Methyl Salicylate (Methyl Salicylate): GB 28355—2012[S]. Beijing: Standards Press of China, 2012.
[11]	National Bureau of Import and Export Commodity Inspection of the People’s Republic of China. Determination of methyl salicylate content in natural wintergreen oil for export-Gas chromatography: SN/T 0513—95[S]. Beijing: Standards Press of China, 1995.
[12]	Wang Yunfeng, Yang Shaoqun. Determination of methyl salicylate in compound Shangfuning cataplasmata by HPLC[J]. Modern Medicine & Health, 2017, 33 (18) : 2772-2774.
[13]	Xu Jia, Cheng Dong, Qian Zhongyi, et al. Determination of three components in compound methyl salicylate and diphenhydramine spray by HPLC[J]. Strait Pharmaceutical Journal, 2018, 30 (2) : 65-68.
[14]	He Xiaorong, Zhang Huan, Tan Xiangshan, et al. Determination of camphor and methylsalicylate in compound camphor cream by HPLC[J]. Central South Pharmacy, 2019, 17 (6) : 872-875.
[15]	Liu Tao, Wu Lin, Yang Ting, et al. Simultaneous determination of menthol and methylis salicylas in tincture spasmodic analgesic by gas chromatography[J]. Chin J of Clinical Rational Drug Use, 2018, 11 (30) : 37-39.
[16]	Dai Gaofei, Jin Jiahua, Luo Tian, et al. Determination of eucalyptol, menthol, methyl salicylate, cinnamylaldehyde and eugenol in Shexiang Qufengshi oil by GC[J]. Chin J Pharm Anal, 2019, 39 (10) : 1821-1827.
[17]	Shen Xiaozhong, Cui Suixu, Qiu Weifen, et al. Simultaneous determination of camphor, menthol and methyl salicylate in dieda zhentong plasters by GC[J]. China Pharmacist, 2020, 23 (4) : 772-774.
[18]	Li Haiyan, Kang Jian, Li Yanchao, et al. Simultaneous determination of salicylate in shangshizhitong adhesive plaster by GC-MS[J]. Pharma J Chin PLA, 2018, 34 (6) : 510-513.
[19]	Zhu Yinghao, Liu Bo, Huang Weihong. Simultaneous determination of 4 kinds of salicylic acid esters in toothpaste by gas chromatography-mass spectrometry[J]. Occup and Health, 2018, 34 (2) : 175-177, 181.
[20]	Pandey B P, Thapa R, Upreti A. Chemical composition, antioxidant and antibacterial activities of essential oil and methanol extract of Artemisia vulgaris and Gaultheria fragrantissima collected from Nepal[J]. Asian Pacific Journal of Tropical Medicine, 2017, 10 (10) : 952-959. doi: 10.1016/j.apjtm.2017.09.005

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

Determination of methyl salicylate in 6 kinds of cosmetics bases by GC

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