液质联用法同时测定化妆品中辛酰羟肟酸、对羟基苯乙酮、p-茴香酸的含量

doi:10.3969/j.issn.2097-2806.2023.05.015

Abstract

Abstract:

The content of caprylhydroxamic acid, 4-hydroxyacetophenone and p-anisic acid in cosmetics was simultaneously determined by HPLC-MS. The mobile phase was 0.1% acetic acid in acetonitrile （containing 0.1% formic acid） by using the gradient elution method. The qualitative analysis of these components was based on the retention time and the relative abundance ratio of the characteristic ion pairs. The peak area of the characteristic ions was used for quantitative analysis. The standard curve method was used to calculate the content of the three substances. The results showed that, in liquid matrix, lotion matrix and cream matrix, caprylhydroxamic acid, 4-hydroxyacetophenone and p-anisic acid showed good linear relationships in the range of 10-2 000, 2-2 000 and 5-2 000 ng/mL, respectively, while the correlation coefficients （r） were>0.999. This method was applied to determine the caprylhydroxamic acid, 4-hydroxyacetophenone and p-anisic acid in cosmetics, the results of which were stable within 48 hours. The recovery rates were between 87.37% and 111.56%. The average relative standard deviation （RSD） of the precision research was 1.4%, 1.8% and 1.6%, respectively. This method is efficient, convenient, and accurate in qualitative and quantitative analysis. It is suitable for quantitative and qualitative analysis of caprylhydroxamic acid, 4-hydroxyacetophenone and p-anisic acid in cosmetics of different matrices.

Key words: HPLC-MS, cosmetics, caprylhydroxamic acid, 4-hydroxyacetophenone, p-anisic acid

CLC Number:

TQ658

Li Zexiaqiong, Qiu Hongyan, Ma Ying, Liu Dan, Zhao Li. Simultaneous determination of caprylhydroxamic acid, 4-hydroxyacetophenone and p-anisic acid in cosmetics by HPLC-MS[J].China Surfactant Detergent & Cosmetics, 2023, 53(5): 596-601.

Figures/Tables 5

Tab. 1

Tab. 2

Fig. 1

Tab. 3

Tab. 4

References 14

[1]	Xiao Shuxiong, Zeng Zijun, Liang Zhuye, et al. Current status and regulatory recommendations for the use of unlisted cosmetic preservatives[J]. Flavour Fragrance Cosmetics, 2020, 180(3): 77-81.
[2]	Sun Liming. Effects of polymers on the rheology profile, sensory profile and moisturizing of cosmetic formulations[J]. Detergent & Cosmetics, 2008(4): 294-295.
[3]	Meng Xiao, Chen Qinsheng, Chen Liang, et al. Safety evaluation and global cosmetic regulations for caprylhydroxamic acid[J]. Detergent & Cosmetics, 2019, 42(12): 18-22.
[4]	National Medical Products Administration. Name List of Used Cosmetic Raw Materials (Version 2021) [EB/OL]. (2021-04-27) [2022-12-09]. https://www.nmpa.gov.cn/directory/web/nmpa/xxgk/ggtg/qtggtg/20210430162707173.html.
[5]	Liu Yuling, Pan Xiaohong, Yin Shuai, et al. Determination of 4-hydroxyacetophenone in cosmetics by ultra performance liquid chromatography[J]. Journal of Food Safety and Quality, 2017, 8(9): 3583-3587.
[6]	Li Chengbei, Dou Jie, Yang Jie. No additive preservative system for cosmetics[J]. Industrial Microbiology, 2016, 46(4): 41-48.
[7]	Mao Qiaoshan, Li Xijun, Zhou Liwu. Determination of 4-hydroxyacetophenone in cosmetics by high performance liquid chromatography[J]. China Surfactant Detergent & Cosmetics, 2018, 48(2): 119-122.
[8]	Kong Qiuchan, Zhang Yi, Liu Wei, et al. Application of a blend of p-anisic acid, sodium levulinate and sodium dehydroacetate in cosmetics[J]. Flavour Fragrance Cosmetics, 2018, 10(5): 45-56.
[9]	Wang Fei. Determination of p-anisic acid in cosmetics by high performance liquid chromatography[J]. Detergent & Cosmetics, 2021, (1): 17-19, 24.
[10]	National Medical Products Administration. Safety and Tchnical Standards for Cometics (Version 2015) [EB/OL]. (2015-12-23) [2022-12-09]. https://www.nmpa.gov.cn/hzhp/hzhpfgwj/hzhpgzwj/20151223120001986.html.
[11]	Name List of Prohibited Raw Materials for Cosmetics[EB/OL]. (2021-05-26)[2022-12-09]. https://www.nmpa.gov.cn/xxgk/ggtg/qtggtg/20210528174051160.html.
[12]	Mao Qiaoshan, Li Xijun, Zhou Liwu. Determination of 4-hydroxyacetophenone in cosmetics by high performance liquid chromatography[J]. China Surfactant Detergent & Cosmetics, 2018, 48(2): 119-122.
[13]	Zhu Liping, Huang Zebin, Li Dong, et al. Method for determination of phenoxyethanol and octanoylhydroxamic acid in cosmetics[J]. Industrial Microbiology, 2021, 51(3): 42-46.
[14]	Fang Yilin, Long Qiuyi, Li Qiuying, et al. Determination of p-hydroxyacetophenone in cosmetics by liquid-mass chromatography[J]. Journal of Inspection and Quarantine, 2020, 30(3): 21-23.

序号	物质名称	电离方式	母离子/（m/z）	Frag./V	子离子/（m/z）	CE/V
1	对羟基苯乙酮	ESI⁺	136.95	23	42.7^*	13
1	对羟基苯乙酮	ESI⁺	136.95	23	94.7	10
2	辛酰羟肟酸	ESI⁺	160.05	29	56.75^*	15
2	辛酰羟肟酸	ESI⁺	160.05	29	103.8	13
3	p-茴香酸	ESI⁺	152.987	22	108.82^*	13
3	p-茴香酸	ESI⁺	152.987	22	93.8	18

物质名称	回归方程	相关系数r	检出限/（ng/mL）	定量限/（ng/mL）	线性范围/（ng/mL）
辛酰羟肟酸	y=1 207x-858	0.999 6	3.16	10.52	10.52~2 094.00
对羟基苯乙酮	y=1 602x+39 442	0.999 5	0.61	2.02	2.02~2 031.97
p-茴香酸	y=1 050x-1 994	0.999 2	1.52	5.06	5.06~2 017.98

成分	加标质量浓度/（ng/mL）	实测平均质量浓度/（ng/mL）			回收率/%
成分	加标质量浓度/（ng/mL）	水基质	乳基质	霜基质	水基质	乳基质	霜基质
辛酰羟肟酸	52.35	47.89	47.87	54.70	91.49	91.45	104.48
		46.85	48.12	53.11	89.50	91.92	101.45
		46.77	48.79	51.46	89.33	93.20	98.31
	523.50	483.52	488.04	472.87	92.36	93.23	90.33
		473.36	461.68	480.75	90.42	88.19	91.83
		466.26	477.29	472.75	89.07	91.17	90.30
	1 047.00	987.57	983.89	962.36	94.32	93.97	91.92
		956.72	1 037.90	971.01	91.38	99.13	92.74
		944.41	960.80	965.01	90.20	91.77	92.17
对羟基苯乙酮	50.80	47.62	48.22	48.52	93.74	94.92	100.62
		48.15	45.03	48.27	94.78	88.64	107.20
		48.27	47.77	48.41	95.02	94.04	101.34
	507.99	501.72	476.47	506.82	98.77	93.80	99.77
		491.40	503.12	496.97	96.73	99.04	97.83
		498.05	505.18	501.67	98.04	99.45	98.76
	1 015.98	892.67	888.64	887.71	87.86	87.47	87.37
		953.15	939.04	932.92	93.82	92.43	91.82
		926.68	945.85	951.00	91.21	93.10	93.60
p-茴香酸	50.45	52.63	55.94	55.28	104.32	110.87	109.58
		55.17	54.33	54.39	109.35	107.68	107.80
		55.61	55.10	56.28	110.22	109.21	111.56
	504.50	451.81	457.93	485.66	89.56	90.77	96.27
		461.64	474.77	472.86	91.50	94.11	93.73
		455.14	448.89	462.62	90.22	88.98	91.70
	1 008.99	1 053.48	937.17	1 008.43	104.41	92.88	99.94
		1 022.13	926.05	1 015.53	101.30	91.78	100.65
		1 007.18	974.35	972.56	99.82	96.57	96.39

[1]	Jingxuan Liu, Jianming Jin, Hua Wu. Botanical cosmetic ingredients （VII）Research and development of plant antifungal [J]. China Surfactant Detergent & Cosmetics, 2024, 54(3): 259-266.
[2]	Wu Bi, Xiaohong Pan, Xiaoqin Tu, Shuai Yin, Hui Sun. Analysis of the mechanism of anti-sensitive skin effect of cosmetic raw material Stephania tetrandra based on network pharmacology [J]. China Surfactant Detergent & Cosmetics, 2024, 54(3): 305-312.
[3]	Yaoyao Li. Study on the anti-aging and antioxidant effects of isosinensetin [J]. China Surfactant Detergent & Cosmetics, 2024, 54(3): 313-319.
[4]	Liyuan Zhang, Linqi Yan, Qiaoyuan Cheng, Lvye Qi, Rong Wang, Liuqian Huang. Determination of 14 kinds of α-hydroxy acids and hydroxy esters in cosmetics [J]. China Surfactant Detergent & Cosmetics, 2024, 54(3): 353-359.
[5]	Wei Xu, Po Zou, Changyu Li, Ming Yang, Yan Lu, Huiliang Li. Determination of 36 stimulants in cosmetics by ultra performance liquid chromatography-tandem mass spectrometry [J]. China Surfactant Detergent & Cosmetics, 2024, 54(3): 360-368.
[6]	Kangfu Zhou, Yixuan Zhi, Feifei Wang, Yazhuo Shang. New emulsion system and its application in cosmetics （VI）Microemulsion [J]. China Surfactant Detergent & Cosmetics, 2024, 54(2): 139-148.
[7]	Zhen Xie, Wei Huang, Jinsong Zhang, Shuhuai Chen, Linji Qu, Rong Kuang. Study on biomarkers of corneal injury in the evaluation of eye irritation of cosmetics [J]. China Surfactant Detergent & Cosmetics, 2024, 54(2): 161-167.
[8]	Xiaohong Pan, Ziqi Gao, Zhen Chen, Shuai Yin, Haiping Huang, Bin Hu. Discussion on the current situation of research and management on the stability of cosmetic products in China [J]. China Surfactant Detergent & Cosmetics, 2024, 54(2): 201-208.
[9]	Li Lu, Fang Fang, Youlong Feng, Ling Cao. Screening for illegal addition of sulfonamides in cosmetic products using ultra-performance liquid chromatographytriple quadrupoletandem mass spectrometry with precursor ion scanning [J]. China Surfactant Detergent & Cosmetics, 2024, 54(2): 216-223.
[10]	Ren Wang, Yuanyang Wu, Jia Qiao, Linqi Yan, Cen Chen, Liyuan Zhang. Study on phenoxyethanol content in children’s cosmetics on the mark and preliminary risk assessment [J]. China Surfactant Detergent & Cosmetics, 2024, 54(2): 224-230.
[11]	Yixiang Lu, Liting Wu, Jimin Jiang, Hailu Chen, Xuan Huang. Determination of tolnaftate and liranaftate in cosmetics by high performance liquid chromatography and verification by high performance liquid chromatography-tandem mass spectrometry [J]. China Surfactant Detergent & Cosmetics, 2024, 54(2): 231-238.
[12]	Liyuan Zhang, Qiaoyuan Cheng, Cen Chen, Zehua Li, Liuqian Huang, Lvye Qi. Determination of 3 kinds of α-hydroxy acids and their esters in cosmetics by high performance liquid chromatography [J]. China Surfactant Detergent & Cosmetics, 2024, 54(1): 102-106.
[13]	Linling Lu, Hui Lu, Chunyan Min, Yefei Qian. Determination of functional components of Glycyrrhizae, Ginseng and Scutellariae in facial masks by UHPLC-MS/MS [J]. China Surfactant Detergent & Cosmetics, 2024, 54(1): 107-113.
[14]	Xu Han, Jiajia Wu, Na Wu, Yazhuo Shang. New emulsion system and its application in cosmetics （V） Janus emulsion [J]. China Surfactant Detergent & Cosmetics, 2024, 54(1): 24-31.
[15]	Feng Liu, Yuanchang Deng, Guohong Ying, Xiaowei Wang. Establishment of duplex-PCR method for rapid detection of Pluralibacter gergoviae [J]. China Surfactant Detergent & Cosmetics, 2024, 54(1): 45-50.

Simultaneous determination of caprylhydroxamic acid, 4-hydroxyacetophenone and p-anisic acid in cosmetics by HPLC-MS

RichHTML

PDF (PC)

Like

Knowledge

Abstract

Cite this article

share this article

Figures/Tables 5

References 14

Related Articles 15

Metrics

Comments

Recommended 10

时间/min	φ（溶液A）/%	φ（溶液B）/%
0	98	2
4	98	2
5	63	37
11	63	37
11.1	98	2
15	98	2