UHPLC-MS/MS法测定面膜化妆品中甘草、人参和黄芩类功效成分

doi:10.3969/j.issn.2097-2806.2024.01.015

Abstract

Abstract:

An analytical method was established for the determination of Glycyrrhizae functional components （liquiritin and glycyrrhizic acid）, Ginseng functional components （ginsenoside Rg1, ginsenoside Rb1, ginsenoside Re） and Scutellariae functional components （baicalin） in facial mask cosmetics with ultra-high performance liquid chromatography triple quadrupole mass spectrometry （UHPLC-MS/MS）. This method was used to monitor the risk of 20 batches of samples sold on the market. The samples were extracted by ultrasonic method using 0.1% formic acid in methanol. The mobile phase was 0.1% formic acid aqueous solution-acetonitrile solution, and the gradient elution was carried out. The samples were separated on the ACQUITY UPLC HSS T₃（2.1 mm×100 mm, 1.8 μm） column and detected by UHPLC-MS/MS negative ion mode. At the same time, the pretreatment conditions and UHPLC-MS/MS conditions were optimized and the method was verified. The results show that the method shows good linearity in the mass concentration range of 0.25-100 ng/mL for liquiritin and baicalin, and 0.50-200 ng/mL for ginsenoside Rg1, ginsenoside Rb1, ginsenoside Re and glycyrrhizic acid, with R no less than 0.998. The limits of detection are in the range of 0.41-6.4 μg/kg （S/N=3）. The average recoveries in the sample matrix of facial masks are from 95.9% to 109.1%, with the relative standard deviations （RSDs） less than 4.9% （n=6）. This method is suitable for the determination of ginseng functional components in the ginseng cosmetics.

Key words: facial masks cosmetics, Glycyrrhizae, Ginseng, Scutellariae, functional components, UHPLC-MS/MS

CLC Number:

TQ658

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.

Figures/Tables 7

Fig. 1

Tab. 1

Fig. 2

Tab. 2

Tab. 3

Tab. 4

Results of the facial mask cosmetic samples claimed to contain Glycyrrhizae, Ginseng and Scutellariae"

序号	名称	标识成分	检出成分	含量	检出成分与标识成分是否一致
1	凝芝水润滋养保湿面膜	甘草酸铵	甘草苷甘草酸	1.99 ng/g 29.88 μg/g	否
2	德胜本草水嫩亮肤透润面膜	甘草酸二钾、甘草根提取物、人参根提取物	甘草苷甘草酸人参皂苷Rg1	25.73 ng/g 108.17 μg/g 检出，低于定量限	是
3	希诺丝大米舒缓面膜	甘草酸二钾	甘草苷甘草酸	3.16 ng/g 221.57 μg/g	否
4	希诺丝黄金亮肤面膜	光果甘草提取物、黄芩根提取物	甘草苷甘草酸黄芩苷	2.53 ng/g 检出，低于定量限 46.53 ng/g	是
5	希诺丝芦荟保湿舒缓面膜	甘草酸二钾	甘草苷甘草酸	83.92 ng/g 162.78 μg/g	否
6	方嗅玻尿酸多肽水光精华蚕丝面膜	甘草根提取物	甘草酸	0.08 μg/g	是
7	八女仙容薰衣草舒缓柔肤面膜	甘草酸二钾	甘草苷甘草酸	6.88 ng/g 267.17 μg/g	否
8	丁家宜烟酰胺水光提亮面膜	甘草酸二钾、光果甘草提取物、黄芩根提取物	甘草苷甘草酸 —	5.43 ng/g 578.93 μg/g —	否
9	兰薇欧墨角藻柔润面膜	甘草酸二钾	甘草酸	200.41 μg/g	是
10	芮朵缤纷蔷薇盈柔面膜	甘草酸二钾	甘草酸	183.06 μg/g	是
11	相宜本草补水面膜	甘草酸二钾	甘草苷甘草酸	检出，低于定量限 287.08 μg/g	否
12	摩肌博士胶原水盈修护面膜	甘草酸二钾	甘草苷甘草酸	2.62 ng/g 1.81 mg/g	否
13	绿叶多肽提拉紧致面膜	甘草酸二钾、光果甘草提取物、黄芩提取物	甘草苷甘草酸 —	1.66 ng/g 206.12 μg/g —	否
14	辣木籽清洁净透黑膜	—	—	—	是
15	欣兰亭芍药靓肤舒缓面膜	—	—	—	是
16	安菲奈尔灵芝青春焕肤面膜	—	—	—	是
17	欣兰亭小分子肽嫩肤面膜	—	—	—	是
18	维他命C盈润焕采面膜	—	—	—	是
19	七分妆水果面膜	—	甘草酸	3.32 μg/g	否
20	悠莱软磷脂源生舒缓面膜	—	甘草酸	0.10 μg/g	否

Tab. 4

Fig. 3

References 15

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编号	物质名称	母离子（m/z）	DP/V	子离子（m/z）	CE/V
1	甘草苷	417.1	-95	255.1^*/135.1	-26/-38
2	黄芩苷	445.1	-50	269.1^*/175.0	-26/-16
3	人参皂苷Rg1	845.5	-150	799.4^*/637.5	-38/-38
4	人参皂苷Rb1	1 153.6	-80	1 107.6^*/945.5	-26/-60
5	人参皂苷Re	991.5	-150	945.5^*/637.5	-40/-55
6	甘草酸	821.1	-120	351.0^*/645.4	-58/-60

物质名称	线性方程	相关系数r	线性范围/ （ng/mL）	检出质量浓度/ （ng/mL）	LOD/ （ng/g）	定量质量浓度/ （ng/mL）	LOQ/ （ng/g）
甘草苷	Y=7.98×10⁴X+1.81×10³	0.999 3	0.27~108.37	0.02	0.42	0.07	1.4
黄芩苷	Y=4.73×10⁴X-1.23×10³	0.999 4	0.26~102.25	0.02	0.41	0.07	1.4
人参皂苷Rg1	Y=9.37×10³X-1.27×10³	0.998 2	0.53~210.90	0.12	2.3	0.39	7.8
人参皂苷Re	Y=1.28×10⁴X+2.99×10³	0.998 4	0.63~250.29	0.09	1.9	0.32	6.3
人参皂苷Rb1	Y=8.23×10³X+1.01×10³	0.998 1	0.63~251.78	0.17	3.4	0.56	11
甘草酸	Y=1.53×10⁴X+3.05×10³	0.999 0	0.45~179.45	0.08	1.6	0.26	5.2

编号	物质名称	加入量/（μg/g）	平均回收率/%	RSD/%
1	甘草苷	0.1，0.5，2.0	106.6，103.9，107.1	1.2，2.5，1.9
2	黄芩苷	0.1，0.5，2.0	105.4，100.3，104.1	2.6，4.1，2.3
3	人参皂苷Rg1	0.2，1.0，4.0	102.5，100.9，105.3	2.6，2.7，0.7
4	人参皂苷Rb1	0.2，1.0，4.0	98.1， 95.9，103.5	3.2，5.3，4.9
5	人参皂苷Re	0.2，1.0，4.0	102.5，101.4，109.1	3.8，4.5，3.0
6	甘草酸	0.2，1.0，4.0	102.9，102.8，112.6	3.2，1.2，3.3

Determination of functional components of Glycyrrhizae, Ginseng and Scutellariae in facial masks by UHPLC-MS/MS

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