UPLC-MS/MS法测定化妆品中5种美白剂

doi:10.3969/j.issn.2097-2806.2024.07.016

Abstract

Abstract:

A method was established for quantitative determination of five whitening agents in cosmetics using ultra-high performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）. The samples were extracted with methanol-water solution （70∶30）, ultrasonic extraction for 30 minutes and then separated by Agilent column （ZORBAX RR StableBond Aq） followed by gradient elution. An electrospray ionization （ESI） source in negative ion mode was utilized for multiple reaction monitoring （MRM） scanning. The results show that under optimal conditions no obvious matrix effect exists in 3 different cosmetic matrices. Among the three cosmetics with different types of matrices, good linearity is obtained for five whitening agents in the range of 1.0-200.0 ng/mL, and the correlation coefficients （R²） are more than 0.996. The limit of detection （LOD） and limit of quantitation （LOQ） are 0.01-0.1 mg/kg and 0.03-0.3 mg/kg, respectively. Spike recovery is performed on three cosmetics at three different spike levels （1, 2, and 10 times of the LOQ）, and the average recovery range is 82.6%-104.8% with a relative standard deviation of 2.1%-8.6% （n=6）. This method is easy to implement, efficient and accurate. It is suitable for quantitative analysis of five whitening agents, including deoxyarbutin, α-arbutin, β-arbutin, hydroquinone, and ursolic acid in common cosmetics, providing technical support for the regulation and risk monitoring of the cosmetics industry.

Key words: UPLC-MS/MS, whitening agents, cosmetics

CLC Number:

TQ658

Changzhao Wang, Zihao Li, Yixin Wang, Yue Yang. Determination of 5 whitening agents in cosmetics using UPLC-MS/MS[J].China Surfactant Detergent & Cosmetics, 2024, 54(7): 873-878.

Figures/Tables 8

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References 16

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步骤	时间/min	流速/（mL/min）	流动相体积分数/%
步骤	时间/min	流速/（mL/min）	A	B
1	0.00	0.3	10	90
2	2.50	0.3	90	10
3	4.00	0.3	90	10
4	4.50	0.3	10	90
5	6.00	0.3	10	90

化合物名称	保留时间/min	母离子（m/z）	子离子（m/z）	去簇电压/ V	碰撞能量/eV
脱氧熊果苷	4.20	193.1	108.1^*	-35	-21
脱氧熊果苷	4.20	193.1	193.1	-35	-5
α-熊果苷	2.72	271.2	108.2^*	-90	-34
α-熊果苷	2.72	271.2	151.2	-90	-16
β-熊果苷	1.86	271.2	108.2^*	-90	-32
β-熊果苷	1.86	271.2	151.2	-90	-17
对苯二酚	3.05	109.1	108.1^*	-75	-21
对苯二酚	3.05	109.1	81.1	-75	-17
熊果酸	4.54	455.6	455.6^*	-16	-10
熊果酸	4.54	455.6	455.6	-16	-10

化合物名称	基质名称	回归方程	线性范围/（ng/mL）	相关系数R²	方法检出限/（mg/kg）	方法定量限/（mg/kg）
脱氧熊果苷	水乳	Y=1.68×10⁵X+8.78×10³	1.0~200.0	0.996 1	0.01	0.03
	膏霜	Y=1.41×10⁵X-6.76×10⁴	1.0~200.0	0.998 2	0.01	0.03
	粉饼	Y=1.50×10⁵X+6.25×10⁴	1.0~200.0	0.997 4	0.01	0.03
α-熊果苷	水乳	Y=1.44×10⁵X-1.10×10⁵	1.0~200.0	0.998 2	0.02	0.06
	膏霜	Y=1.01×10⁵X+5.46×10⁴	1.0~200.0	0.997 1	0.02	0.06
	粉饼	Y=1.211×10⁵X-1.02×10⁵	1.0~200.0	0.997 5	0.02	0.06
β-熊果苷	水乳	Y=1.34×10⁵X+3.46×10⁵	1.0~200.0	0.998 8	0.05	0.15
	膏霜	Y=1.51×10⁴X+1.53×10⁴	1.0~200.0	0.997 6	0.05	0.15
	粉饼	Y=1.01×10⁴X-1.33×10⁴	1.0~200.0	0.998 4	0.05	0.15
对苯二酚	水乳	Y=8.37×10⁴X-2.27×10⁴	1.0~200.0	0.998 6	0.05	0.15
	膏霜	Y=9.87×10⁴X+8.35×10³	1.0~200.0	0.999 1	0.05	0.15
	粉饼	Y=7.00×10⁴X+6.00×10³	1.0~200.0	0.997 6	0.05	0.15
熊果酸	水乳	Y=6.02×10⁴X+5.26×10³	1.0~200.0	0.999 2	0.1	0.3
	膏霜	Y=5.22×10⁴X-1.56×10³	1.0~200.0	0.998 5	0.1	0.3
	粉饼	Y=4.13×10⁴X+2.12×10³	1.0~200.0	0.999 0	0.1	0.3

样品名称	添加水平/ （mg/kg）	水乳		膏霜		粉饼
样品名称	添加水平/ （mg/kg）	回收率/%	RSD/%	回收率/%	RSD/%	回收率/%	RSD/%
脱氧熊果苷	0.03	91.8	4.2	87.6	6.8	84.5	7.6
	0.06	92.4	4.6	93.0	4.5	85.8	6.7
	0.30	95.0	3.1	100.4	3.4	90.3	5.5
α-熊果苷	0.06	90.6	6.5	92.1	6.8	88.5	8.6
	0.12	97.0	5.1	90.5	5.4	87.0	5.5
	0.60	92.8	2.5	98.6	5.2	89.9	4.4
β-熊果苷	0.15	88.3	5.6	88.7	7.5	82.6	5.0
	0.30	88.9	4.2	93.4	4.4	85.6	4.7
	1.50	90.4	3.2	99.6	2.1	90.5	3.6
对苯二酚	0.15	89.9	6.5	93.2	5.4	84.6	5.7
	0.30	91.7	4.4	90.8	3.4	88.9	4.8
	1.50	92.3	3.3	104.8	2.0	87.5	3.0
熊果酸	0.3	95.2	5.6	86.9	4.5	91.0	5.5
	0.6	91.3	4.2	89.5	4.0	91.1	3.4
	3.0	97.8	2.9	99.5	2.7	92.4	3.1

Determination of 5 whitening agents in cosmetics using UPLC-MS/MS

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