UPLC-ESI-Q-TOF/MS法测定化妆品中倍他米松及其8种类似物

doi:10.3969/j.issn.1001-1803.2022.02.014

Abstract

Abstract:

A method of ultra-performance liquid chromatography-high resolution mass spectrometry （UPLC-ESI-Q-TOF/MS） was developed for simultaneous determination of betamethasone and its 8 analogues. The separation was executed on a small particle column, and gradient elution was used. The mass spectrometer was performed in positive ion mode, and the identification was performed by MS² scan with aid of standards, and the determination was carried out in MS scan mode by the external standard method. The analysis method developed was validated. The linear relationship in the linear range was satisfactory, the detection limit was between 0.05 and 0.34 mg/kg. The recovery was 93.1%-103.7%, and the relative standard deviation was less than 6%. In the analysis of 10 batches of cosmetics, glucocorticoids were detected in five batches. Furthermore, two glucocorticoids additives were found for the first time, i.e., betamethasone 17-propionate and betamethasone 21-propionate.

Key words: UPLC-ESI-Q-TOF/MS, cosmetics, glucocorticoid

CLC Number:

TQ658

Jia Changping,Zhang Bin,Zhang Shanshan,Zheng Jiaxin,Zheng Mei,Chen Wei. Determination of betamethasone and eight analogues in cosmetics by UPLC-ESI-Q-TOF/MS[J].China Surfactant Detergent & Cosmetics, 2022, 52(2): 207-213.

Figures/Tables 11

Fig.1

Fig.2

Fig.3

Tab. 1

Tab. 2

Tab. 3

Tab. 4

Tab. 5

Fig.4

Fig.5

Fig.6

References 13

[1]	Yang Yanwei, Liu Siran, Zhang Weiqiang, et al. Investigation of substances prohibited in cosmetic products[J]. Journal of Environment and Health, 2017, 34(1): 48-52.
[2]	Zhao Hua. Damage and detection of illegally added hormone in cosmetics[J]. Detergent & Cosmetics, 2016, 39(3): 8-10.
[3]	China Food and Drug Administration. Safety and Technical Standards for Cosmetics (2015 Edition)[S]. Beijing: People’s Medical Publishing House, 2017.
[4]	Zhu Fuqiang, He Zhiqiao, He Qian, et al. Research progress on liquid chromatography-tandem mass spectrometry applied in cosmetic quality and safety analysis[J]. Flavour Fragrance Cosmetics, 2019 (3): 75-79.
[5]	Fan Xiaolong, Wu Wanqin, Huang Kun, et al. Rapid determination of glucocorticoids in cosmetics by QuEChERS-ultra performance liquid chromatography tandem mass spectrometry[J]. Journal of Food Safety and Quality, 2021, 12(1): 86-93.
[6]	Dong Yalei, Liu Zhao, Wang Haiyan, et al. Determination of 43 glucocorticoids in infant eczema products by UHPLC-MS/MS[J]. China Surfactant Detergent & Cosmetics, 2020, 50(12): 885-895.
[7]	Zhang Jing, Yan Xiaohong, Lai Junmin, et al. Simultaneous detection of 3 other standard glucocorticoids illegally added in cosmetics by liquid chromatography-tandem mass spectrometry[J]. Pharmacy Today, 2018, 28(11): 733-735.
[8]	Weng Donghai, Liu Jiang, Jiang Qingqing, et al. A new illegal addition of glucocorticoids in cosmetics: betamethasone butyrate acetate[J]. Flavour Fragrance Cosmetics, 2019 (3): 45-49.
[9]	Hu Bei, Li Lixia, Liu Hong, et al. Simultaneous determination of 35 sex hormones in cosmetics by ultra-performance liquid chromatography-tandem mass spectrometry[J]. Journal of Instrumental Analysis, 2020, 39(8): 986-992.
[10]	General Administration of Quality Supervision, Inspection and Quarantine. Determination of 41 glucocorticoids in cosmetics-LC-MS/MS and TLC method: GB/T 24800—2009[S]. Beijing: China Quality and Standards Publishing&Media Co., Ltd., 2009.
[11]	Luo Huitai, Huang Xiaolan, Wu Huiqin, et al. High throughput screening of 86 kinds of glucocorticoids in cosmetics using QuEChERS and isotope dilution-liquid chromatography copuled to high resolution time-of-flight mass spectrometry[J]. Chinese Journal of Analytical Chemistry, 2017, 45(9): 1381-1388.
[12]	Liu Hong, Yang Piaopiao, Li Lixia. Detection of 73 glucocorticoids in cosmetics by ultra performance liquid chromatography-tandem mass spectrometry with pass-through column purification[J]. Journal of Instrumental Analysis, 2020, 39(9): 1112-1119.
[13]	Luo Huitai, Huang Xiaolan, Wu Huiqin, et al. Simultaneous determination of 53 kinds of glucocorticoids illegally added in facial mask cosmetics by solid-phase extraction with liquid chromatography-tandem mass spectrometry[J]. Journal of Instrumental Analysis, 2016, 35(2): 119-126.

化合物	分子式	R_t/min	[M+H]⁺	主要子离子
BM	C₂₂H₂₉FO₅	9.362	393.208 1	373.201 1, 355.189 9, 337.180 1, 319.169 6, 279.173 7, 237.127 1, 147.080 2
DXM	C₂₂H₂₉FO₅	9.777	393.208 1	373.201 6, 355.190 6, 337.179 0, 319.167 5, 291.173 8, 237.127 8, 147.079 4
17-DXMP	C₂₅H₃₃FO₆	12.766	449.233 1	429.226 0, 355.189 9, 337.180 0, 319.168 2, 291.174 0, 279.174 2, 153.089 8, 147.080 6
BMA	C₂₄H₃₁FO₆	12.835	435.217 8	415.210 6, 397.200 1, 379.189 6, 355.190 4, 337.179 8, 319.169 9, 309.184 3, 291.174 6, 279.174 6, 147.080 5
DXMA	C₂₄H₃₁FO₆	13.133	435.217 8	415.213 8, 397.201 3, 379.192 5, 355.189 7, 337.180 7, 319.169 3, 309.186 3, 291.174 6, 237.129 2, 147.079 3
17-BMP	C₂₅H₃₃FO₆	13.225	449.233 1	355.190 7, 337.179 5, 319.168 7, 301.156 5, 291.172 8, 279.174 5, 263.143 5, 147.080 4
21-BMP	C₂₅H₃₃FO₆	13.801	449.233 1	429.229 2, 411.215 4, 393.205 6, 373.200 0, 355.189 9, 337.179 3, 319.168 6, 309.184 1, 291.173 1, 279.173 3, 147.081 0, 57.033 7
21-DXMP	C₂₅H₃₃FO₆	14.093	449.233 1	429.228 1, 411.217 4, 393.206 8, 373.200 6, 355.191 0, 337.180 2, 327.195 5, 319.168 7, 309.184 4, 291.174 0, 237.126 9, 147.080 1, 57.034 1
BMDP	C₂₈H₃₇FO₇	15.992	505.261 4	485.251 1, 411.217 2, 393.204 7, 355.189 8, 337.179 8, 319.169 9, 309.184 4, 301.160 1, 291.175 3, 279.175 2, 153.090 3, 57.033 3

化合物	线性范围/（μg/mL）	线性方程	相关系数r	检出限/（mg/kg）	定量限/（mg/kg）
BM	0.2~10	Y=224X+45 843	0.999 4	0.30	0.98
DXM	0.2~10	Y=223X+38 615	0.999 5	0.34	1.12
17-DXMP	0.2~10	Y=321X+79 377	0.997 8	0.06	0.21
BMA	0.2~10	Y=187X+45 046	0.999 2	0.06	0.19
DXMA	0.2~10	Y=185X+36 189	0.999 4	0.09	0.30
17-BMP	0.2~10	Y=247X+36 166	0.999 3	0.06	0.19
21-BMP	0.2~10	Y=208X+48 504	0.999 1	0.06	0.21
21-DXMP	0.2~10	Y=306X+73 529	0.999 1	0.05	0.17
BMDP	0.2~10	Y=250X+20 969	0.999 7	0.07	0.23

化合物	保留时间/min	RSD/%	平均回收率/%	RSD/%
BM	9.337	2.2	96.2	1.7
DXM	9.612	2.0	96.5	0.7
17-DXMP	12.755	0.1	103.7	5.2
BMA	12.823	0.1	97.3	0.5
DXMA	13.059	0.9	98.0	1.6
17-BMP	13.217	0.1	96.5	0.6
21-BMP	13.795	0.1	96.2	0.9
21-DXMP	14.070	0.1	93.1	3.5
BMDP	15.976	0.1	95.3	0.9

化合物	保留时间/min	RSD/%	峰面积	RSD/%
BM	9.244	0.2	1 225 531	0.8
DXM	9.666	0.2	1 207 812	1.2
17-DXMP	12.733	0.1	1 837 828	1.0
BMA	12.798	0.1	1 035 126	1.0
DXMA	13.084	0.1	1 011 937	0.9
17-BMP	13.195	0.1	1 336 494	0.7
21-BMP	13.763	0.1	1 148 433	1.1
21-DXMP	14.043	0.1	1 667 113	1.0
BMDP	15.931	0.1	1 320 455	0.8

序号	样品名称（标示）	剂型	检出物质	含量/ （mg/kg）
1	保湿面膜	面膜	—	—
2	百草藓方	水剂	17-BMP 21-BMP	49.1 15.3
3	蚕丝面膜	面膜	BM	4.6
4	亮肤霜	霜剂	DXM	22.4
5	祛斑精华液	水剂	—	—
5	防晒霜	霜剂	DXM	12.9
6	美颜霜	霜剂	DXM	3.0
7	护肤乳	乳剂	—	—
8	洁面乳	乳剂	—	—
9	修护祛痘膏	霜剂	—	—
10	收敛爽肤水	水剂	—	—

Determination of betamethasone and eight analogues in cosmetics by UPLC-ESI-Q-TOF/MS

RichHTML

PDF (PC)

Like

Knowledge

Abstract

Cite this article

share this article

Figures/Tables 11

References 13

Related Articles 15

Metrics

Comments

Recommended 10

[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.