UPLC-MS/MS法测定美白化妆品中10种植物原料指标性成分

doi:10.3969/j.issn.2097-2806.2025.04.016

Abstract

Abstract:

A method for simultaneous determination of 10 indicative components from plant materials in whitening cosmetics by ultra-high performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） was established. The sample was extracted by ultrasonic extraction using 80% methanol, then separated on a Phenomenex Kinetex F5 column （3.0 mm×100 mm, 2.6 μm） by gradient elution using 0.1% formic acid solution and acetonitrile as the mobile phases. The mass spectrometry was detected using electrospray ionization source （ESI）, positive and negative ion simultaneous scanning and multiple reaction monitoring （MRM） mode. The results show that there are good linear relationships for 10 indicative components in their respective mass concentration rangers with the correlation coefficients （r） larger than 0.99. The limits of detection （LOD） are in the ranges of 0.07-1.93 μg/kg and the limits of quantitation （LOQ） are in the ranges of 0.22-6.42 μg/kg. The recoveries of toner, cream, emulsion and mask samples at three spiked levels for 10 indicative components are 80.5%-122.5%, with the relative standard deviations （RSD） of 1.3%-10.1% （n=6）. With the advantages of accuracy, high sensitivity and simplicity, this method is suitable for qualitative identification and quantitative analysis of various indicative components from plant materials in various matrix types of whitening cosmetics.

Key words: UPLC-MS/MS, whitening cosmetics, plant materials, indicative components

CLC Number:

TQ658

Weidong Huang. Determination of 10 indicative components from plant materials in whitening cosmetics by UPLC-MS/MS[J].China Surfactant Detergent & Cosmetics, 2025, 55(4): 531-538.

Figures/Tables 7

Tab. 1

Fig. 1

Tab. 2

Tab. 3

Linear ranges, regression equations, correlation coefficients （r）, limits of detection （LODs） and limits of quantification （LOQs） of 10 indicative components in different matrices"

化合物	线性范围/（μg/L）	基质类型	线性回归方程	相关系数（r）	检出限/（μg/kg）	定量限/（μg/kg）
咖啡因	0.05~2.00	水基类	y=2.28×10⁵x+7.27×10⁴	0.998 3	0.43	1.43
		膏霜类	y=2.85×10⁵x+7.77×10⁴	0.995 1	0.37	1.22
		乳液类	y=1.05×10⁵x+1.14×10⁵	0.994 1	0.33	1.09
		面膜类	y=3.34×10⁵x+1.17×10⁵	0.995 1	0.28	0.95
苦参碱	0.05~2.00	水基类	y=1.96×10⁵x-715	0.997 6	0.31	1.02
		膏霜类	y=1.43×10⁵x-1.79×10³	0.991 0	0.41	1.37
		乳液类	y=8.33×10⁴x+662	0.996 7	0.38	1.27
		面膜类	y=1.87×10⁵x-951	0.998 0	0.28	0.94
丹参酮Ⅰ	0.02~1.00	水基类	y=1.66×10⁶x+5.35×10⁴	0.996 4	0.07	0.22
		膏霜类	y=5.37×10⁵x+743	0.994 7	0.22	0.72
		乳液类	y=1.68×10⁵x+5.00×10³	0.997 3	0.18	0.61
		面膜类	y=1.69×10⁶x+1.41×10³	0.997 9	0.11	0.37
丹参酮ⅡA	0.02~1.00	水基类	y=3.69×10⁶x+3.98×10⁴	0.998 2	0.25	0.82
		膏霜类	y=1.06×10⁶x-6.08×10³	0.996 6	0.29	0.96
		乳液类	y=9.86×10⁵x+2.41×10⁴	0.995 7	0.17	0.55
		面膜类	y=2.61×10⁶x-1.44×10⁴	0.997 9	0.12	0.40
没食子酸	0.2~10.0	水基类	y=9.97×10⁴x-1.51×10⁴	0.997 3	1.93	6.42
		膏霜类	y=3.48×10⁵x+1.28×10³	0.995 7	1.42	4.73
		乳液类	y=1.40×10⁵x+3.49×10⁴	0.996 8	1.89	6.31
		面膜类	y=2.02×10⁵x-9.79×10³	0.997 7	1.61	5.36
阿魏酸	0.05~2.00	水基类	y=1.02×10⁵x-155	0.997 7	0.25	0.83
		膏霜类	y=5.16×10⁴x-681	0.995 2	0.63	2.11
		乳液类	y=9.14×10⁴x-61.1	0.997 1	0.25	0.83
		面膜类	y=5.30×10⁴x+351	0.996 4	0.48	1.60
迷迭香酸	0.01~0.50	水基类	y=1.43×10⁵x+94.3	0.996 8	0.11	0.35
		膏霜类	y=1.69×10⁵x+521	0.995 5	0.13	0.44
		乳液类	y=1.26×10⁵x+28.4	0.995 8	0.16	0.54
		面膜类	y=1.79×10⁵x-103	0.998 7	0.10	0.34
芦荟苷	0.02~1.00	水基类	y=1.12×10⁵x+407	0.998 2	0.18	0.59
		膏霜类	y=1.28×10⁵x-2.64×10³	0.994 7	0.23	0.75
		乳液类	y=1.32×10⁵x-51.6	0.996 7	0.21	0.69
		面膜类	y=1.31×10⁵x-722	0.998 0	0.16	0.53
芍药苷	0.01~0.50	水基类	y=6.17×10⁴x+97.0	0.997 1	0.15	0.51
		膏霜类	y=7.59×10⁴x+16.6	0.992 1	0.14	0.47
		乳液类	y=6.30×10⁴x+516	0.997 6	0.16	0.53
		面膜类	y=8.75×10⁴x-66.5	0.998 3	0.09	0.31
三七皂苷R1	0.1~5.0	水基类	y=4.61×10³x+259	0.991 8	1.40	4.68
		膏霜类	y=1.11×10⁴x-130	0.995 3	0.73	2.45
		乳液类	y=5.02×10³x-167	0.994 4	1.26	4.18
		面膜类	y=6.64×10³x+733	0.991 3	1.36	4.53

Tab. 3

Tab. 4

Tab. 5

Identified components and determination results in real samples"

序号	产品名称	标识成分	检测结果
1	××牌美白保湿柔肤水	库拉索芦荟叶提取物	芦荟苷（<LOQ）
2	××牌耀白淡斑精华液	芍药根提取物；丹参根提取物；三七根提取物	芍药苷（ND）；丹参酮Ⅰ（ND）；丹参酮ⅡA（ND）；三七皂苷R1（ND）
3	××牌新源焕白亮肤水	茶叶提取物	咖啡因（ND）；没食子酸（ND）
4	××牌新源焕白亮肤霜	圆叶当归提取物；茶叶提取物	阿魏酸（<LOQ）；咖啡因（ND）；没食子酸（ND）
5	××牌雪莲美白淡斑晚安霜	茶叶提取物；当归根提取物；三七根提取物；芍药根提取物	咖啡因（16.70 μg/kg）；没食子酸（<LOQ）；阿魏酸（ND）；三七皂苷R1（ND）；芍药苷（39.97 μg/kg）
6	××牌祛痘修复膏	丹参根提取物；茶叶提取物	丹参酮Ⅰ（ND）；丹参酮ⅡA（ND）；咖啡因（ND）；没食子酸（<LOQ）
7	××牌璀璨靓肤美白露	茶叶提取物；迷迭香提取物	咖啡因（ND）；没食子酸（<LOQ）；迷迭香酸（ND）
8	××牌复颜晶白凝皙盈润乳	芍药根提取物；东当归根提取物	芍药苷（2.44 μg/kg）；阿魏酸（ND）
9	××牌水光亮白精华乳液	库拉索芦荟叶汁粉	芦荟苷（1.54 μg/kg）
10	××牌雪莲美白淡斑修护乳	茶叶提取物；当归根提取物；三七根提取物；芍药根提取物	咖啡因（ND）；没食子酸（<LOQ）；阿魏酸（<LOQ）；三七皂苷R1（ND）；芍药苷（0.89 μg/kg）
11	××牌肌源奢白晶采雪肌乳	苦参根提取物	苦参碱（17.48 μg/kg）
12	××牌白皙清透面膜	库拉索芦荟叶提取物	芦荟苷（ND）
13	××牌水嫩倍现盈采精华面膜	苦参根提取物；库拉索芦荟叶提取物	苦参碱（22.46 μg/kg）；芦荟苷（ND）
14	××牌蛋白灯泡肌面膜	迷迭香提取物	迷迭香酸（ND）
15	××牌密集补水面膜	茶叶提取物；迷迭香叶提取物	咖啡因（ND）；没食子酸（<LOQ）；迷迭香酸（<LOQ）

Tab. 5

Fig. 2

References 19

[1]	胡积东, 王海瑞. 植物化妆品的研究进展[J]. 香料香精化妆品, 2023(3): 121-124.
[2]	李雪, 王艳萍, 杨兆均, 等. 2014—2021年含植物原料的国产普通化妆品现状分析[J]. 日用化学工业, 2022, 52(8): 875-881.
[3]	周苗苗, 刘睿, 李正. 基于文献计量学分析2012—2022年植物原料化妆品[J]. 香料香精化妆品, 2024(1): 17-20, 107.
[4]	顾宇翔, 刘恕, 周羽. 化妆品原料标准现状及缺失分析[J]. 日用化学工业, 2023, 53(6): 673-678.
[5]	顾宇翔, 周泽琳, 杨轶眉, 等. 高效液相色谱法测定化妆品中黄芩甙[J]. 理化检验(化学分册), 2012, 48(4): 442-444, 448.
[6]	陆军, 李莹. 高效液相色谱法测定化妆品中7种甘草成分[J]. 理化检验-化学分册, 2015, 51(5): 655-658.
[7]	方继辉, 唐国辉, 陈张好. 反相高效液相色谱法同时测定化妆品中甘草苷和甘草酸的含量[J]. 香料香精化妆品, 2015(1): 56-57, 73.
[8]	高俊飞, 朱荃, 段婷婷, 等. 超高效液相色谱测定化妆品中11种植物美白成分[J]. 日用化学工业, 2019, 49(7): 480-484.
[9]	谢文缄, 熊小婷, 席绍峰, 等. 超高效液相色谱-四极杆串联飞行时间质谱法鉴定育发化妆品中4种植物功效成分[J]. 分析测试学报, 2016, 35(2): 164-171.
[10]	席绍峰, 李慧勇, 谭建华, 等. SPE-UPLC-Q-TOF MS测定育发化妆品中人参和甘草类功效成分[J]. 质谱学报, 2015, 36(4): 341-349. doi: 10.7538/zpxb.youxian.2015.0022
[11]	董亚蕾, 乔亚森, 王启林, 等. UHPLC-MS/MS法测定甘草类化妆品中光甘草定的研究[J]. 日用化学工业, 2021, 51(2): 161-165.
[12]	赵晓亚, 林雁飞, 胡小钟, 等. 气相色谱-质谱法同时测定化妆品中5种香豆素类化合物[J]. 分析试验室, 2010, 29(3): 76-79.
[13]	韩晶, 许勇, 郑荣. 化妆品配方中含万寿菊花提取物的α-三联噻吩的测定[J]. 香料香精化妆品, 2022(4): 37-40.
[14]	袁莹莹, 于新兰, 乔亚森, 等. 高效液相色谱-串联质谱法测定化妆品中红景天提取物[J/OL]. 分析试验室. http://kns.cnki.net/kcms/detail/11.2017.TF.20231109.1245.016.
[15]	张会亮, 程琳, 黄传峰, 等. 植物组方美白类化妆品宣称芍药成分的真实性分析[J]. 香料香精化妆品, 2020(5): 37-39, 45.
[16]	邓映明, 陈媛, 邓美凌, 等. 液质联用法测定甘草组方化妆品中4种标志性成分[J]. 日用化学工业, 2021, 51(12): 1278-1282.
[17]	张伟清, 侯俐南, 李彬, 等. 超高效液相色谱-串联质谱法(UPLC/MS-MS)测定人参化妆品中人参功效成分[J]. 日用化学工业, 2021, 51(6): 577-582.
[18]	袁莹莹, 董亚蕾, 乔亚森, 等. 高效液相色谱-串联质谱法测定化妆品中积雪草的4种活性成分[J]. 分析化学, 2022, 50(12): 1899-1906.
[19]	曹梅荣, 马俊美, 王娟, 等. 高效液相色谱-串联质谱法测定化妆品中10种生物碱[J]. 色谱, 2019, 37(9): 977-982. doi: 10.3724/SP.J.1123.2019.01054

化合物	母离子/（m/z）	子离子/（m/z）	CE/V	DP/V
咖啡因	195.1	138.1^*；110.0	27；32	80
苦参碱	249.1	148.2^*；150.2	45；43	80
丹参酮Ⅰ	277.1	249.2^*；178.2	30；52	80
丹参酮ⅡA	295.1	277.2^*；249.2	28；33	80
没食子酸	169.0	125.0^*；79.0	-20；-30	-70
阿魏酸	193.0	134.1^*；178.1	-23；-18	-50
迷迭香酸	359.1	161.0^*；197.0	-24；-25	-50
芦荟苷	417.2	297.1^*；268.0	-28；-48	-160
芍药苷	525.2	449.1^*；121.1	-20；-35	-30
三七皂苷R1	977.5	931.6^*；637.6	-38；-60	-50

化合物	基质效应/%
化合物	水基类	膏霜类	乳液类	面膜类
咖啡因	45.5	51.2	50.7	68.0
苦参碱	61.5	54.0	47.0	69.3
丹参酮Ⅰ	87.7	11.1	35.2	77.0
丹参酮ⅡA	84.7	34.7	33.7	67.7
没食子酸	82.9	77.5	134.7	97.1
阿魏酸	78.4	68.0	42.2	41.2
迷迭香酸	84.8	74.8	69.7	93.5
芦荟苷	81.7	89.8	83.8	77.8
芍药苷	65.5	74.4	84.6	82.8
三七皂苷R1	52.2	51.0	103.2	71.8

化合物	加标质量浓度/（ng/mL）	水基类		膏霜类		乳液类		面膜类
化合物	加标质量浓度/（ng/mL）	回收率/%	RSD/%	回收率/%	RSD/%	回收率/%	RSD/%	回收率/%	RSD/%
咖啡因	0.1	117.2	7.0	108.6	8.8	111.4	7.1	111.3	7.8
	0.2	110.3	6.1	110.8	6.4	106.2	6.7	109.8	8.3
	1.0	103.1	3.9	103.4	5.8	102.6	3.5	108.5	5.6
苦参碱	0.1	103.8	5.0	98.6	4.1	112.7	4.8	82.6	7.3
	0.2	99.2	2.9	82.3	7.2	95.9	7.1	91.2	4.7
	1.0	105.1	2.5	87.2	5.3	114.3	4.6	80.5	2.4
丹参酮Ⅰ	0.05	88.2	6.1	85.3	3.2	81.9	6.2	88.7	5.2
	0.1	88.0	5.5	91.9	7.6	93.2	6.7	97.2	8.3
	0.5	90.2	2.9	89.5	4.5	95.4	4.4	95.5	2.7
丹参酮ⅡA	0.05	95.1	6.4	107.3	8.6	87.2	4.9	115.8	5.6
	0.1	94.3	6.0	103.9	5.0	91.9	6.4	109.5	3.2
	0.5	97.8	4.0	100.3	1.8	96.6	2.0	98.4	2.3
没食子酸	0.5	115.1	7.5	96.3	10.1	118.2	9.4	105.4	9.1
	1.0	110.0	6.3	106.5	7.1	97.4	4.7	94.3	6.0
	5.0	98.1	3.3	88.8	8.3	99.5	7.9	95.4	8.2
阿魏酸	0.1	105.0	7.1	107.2	4.2	92.1	4.6	102.7	8.6
	0.2	109.4	5.6	113.3	3.8	115.0	3.7	96.3	6.4
	1.0	95.8	2.5	107.0	2.9	98.8	5.1	100.4	4.1
迷迭香酸	0.02	113.2	9.6	113.8	2.4	116.1	5.1	122.5	7.4
	0.05	100.3	2.2	107.0	4.5	113.6	4.7	116.9	5.8
	0.2	101.6	3.4	94.1	3.2	96.7	4.5	103.3	6.9
芦荟苷	0.05	109.2	5.4	102.5	7.6	102.5	3.1	118.7	7.9
	0.1	105.4	4.8	103.3	5.2	107.1	3.3	120.6	6.6
	0.5	107.4	4.8	99.8	2.6	106.7	1.9	109.8	4.9
芍药苷	0.02	87.2	3.8	105.4	2.6	90.6	5.3	93.1	8.2
	0.05	94.2	1.9	116.0	3.7	96.2	2.7	107.5	3.6
	0.2	100.8	6.4	96.5	4.2	104.6	5.1	98.8	1.3
三七皂苷R1	0.2	95.2	5.9	90.3	8.2	116.6	9.5	103.8	7.7
	0.5	100.2	4.1	96.9	2.7	101.6	6.1	105.4	8.6
	2.0	106.1	1.5	86.9	3.4	112.5	4.6	120.3	4.1

Determination of 10 indicative components from plant materials in whitening cosmetics by UPLC-MS/MS

RichHTML

PDF (PC)

Like

Knowledge

Abstract

Cite this article

share this article

Figures/Tables 7

References 19

Related Articles 15

Metrics

Comments

Recommended 10

[1]	Qiuyan Zhang, Juntao Liao, Weiwei Liang, Fang Huang, Huiqin Wu, Huitai Luo. Determination of 14 thiazides in cosmetics by ultra high performance liquid chromatography-tandem mass spectrometry [J]. China Surfactant Detergent & Cosmetics, 2025, 55(1): 117-124.
[2]	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.
[3]	Ning Li, Ennian Li, Hongbo Chen, Fang Cheng, Hengfang Zou, Hongpeng Chen. Advances of functional components in whitening cosmetic [J]. China Surfactant Detergent & Cosmetics, 2024, 54(1): 80-89.
[4]	Zhang Xin,Huo Yongli. Determination of eight organic acids such as lactobionic acid in cosmetics by ultra performance liquid chromatography-tandem mass spectrometry [J]. China Surfactant Detergent & Cosmetics, 2023, 53(8): 981-988.
[5]	Liu Zhen, Wang Yumei, Yang Junli, Sun Xiaojie. Determination of 13 bisphenols and alkylphenols environmental hormones in essential oil cosmetics by UPLC-MS/MS method [J]. China Surfactant Detergent & Cosmetics, 2023, 53(7): 826-832.
[6]	Zheng Jiaxin, Jia Changping, Zhang Shanshan. Determination of 29 anti-allergy drugs by UPLC-MS/MS in cosmetics [J]. China Surfactant Detergent & Cosmetics, 2023, 53(7): 833-840.
[7]	Chen Guijuan, Xing Haiyan, Yao Xinyue, Han Yonghong, Tao Juan. Determination of 17 sulfonamides in anti-acne cosmetics with different substrates by UPLC-MS/MS [J]. China Surfactant Detergent & Cosmetics, 2023, 53(4): 487-492.
[8]	Zhang Yanping, Zhou Zongzhou, Huang Wanfeng, Chen Yihua, Zhang Min, He Zuomin. Determination of 16 coumarin compounds in commonly cosmetics plant extract raw materials by UPLC-MS/MS [J]. China Surfactant Detergent & Cosmetics, 2023, 53(2): 226-232.
[9]	Li Xue,Wang Yanping,Yang Zhaojun,Han Jiabing,Li Wen,Hu Fangdi. Analysis of domestic general cosmetics containing plant materials from 2014 to 2021 [J]. China Surfactant Detergent & Cosmetics, 2022, 52(8): 875-881.
[10]	Yan Jun,Wang Rong,Li Zehua,Zhang Liyuan,Cheng Qiaoyuan,Yan Linqi. Simultaneous determination and usage analysis of six functional ingredients in whitening cosmetics [J]. China Surfactant Detergent & Cosmetics, 2022, 52(7): 791-796.
[11]	Xu Xiaohui,Wang Xiaoqiao,Zhao Bo,Du Ruihu,Zhang Hongyan,Shi Xiaofeng. Filtered solid phase extraction-UPLC-MS/MS for determination of 35 glucocorticoids in hair-rearing solutions [J]. China Surfactant Detergent & Cosmetics, 2022, 52(4): 444-450.
[12]	Hu Bei,Li Lixia,Liu Hong,Huang Wei,Ding Xiaoping. Determination of 39 sex hormones in oil-based cosmetics by ultra-performance liquid chromatography-tandem mass spectrometry [J]. China Surfactant Detergent & Cosmetics, 2022, 52(3): 328-336.
[13]	Lu Linling,Qian Yefei,Zhang Bin,Lu Hui,Chen Libo,Min Chunyan,Chen Wei. Determination of 38 anti-infective drugs in cosmetics by ultra high performance liquid chromatography-tandem mass spectrometry [J]. China Surfactant Detergent & Cosmetics, 2022, 52(2): 214-223.
[14]	Ren Qianqian,Wu Hua,Jin Jianming. Botanical cosmetic ingredient (IV) Research and development of skin whitening ingredients from plant extracts with melanogenesis signaling pathway inhibiting effect [J]. China Surfactant Detergent & Cosmetics, 2021, 51(7): 590-597.
[15]	YANG Piao-piao,LIU Hong,LI Li-xia. Detection of 76 glucocorticoids in cosmetics by automatic solid-phase extraction and LC/MS/MS [J]. China Surfactant Detergent & Cosmetics, 2021, 51(5): 468-476.