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

doi:10.3969/j.issn.1001-1803.2021.06.016

摘要/Abstract

摘要：

建立了超高效液相色谱-三重四级杆质谱法（UPLC/MS-MS）测定人参化妆品中人参功效成分（人参皂苷Rg1,人参皂苷Re）,并用该方法对市售28批样品进行风险监测。样品采用甲醇超声提取法,以0.05%甲酸水溶液-0.05%甲酸乙腈溶液为流动相,梯度洗脱,ACQUITY UPLC BEH C₁₈ （2.1 mm×100 mm×1.7 μm）色谱柱分离,以UPLC/MS-MS负离子模式检测。同时对样品前处理条件及色谱-质谱条件进行优化,并完成方法学验证。结果表明,两种目标化合物在0.1~50 ng/mL及0.5~200 ng/mL质量浓度范围内呈良好线性关系,R²大于0.999 6;LOD为0.001 7~0.003 0 μg/g （S/N=3）;在膏霜、乳液、洗护类基质中加标回收率为81.87%~94.45%,相对标准偏差小于5.64% （n=6）。该方法适用于人参化妆品中人参功效成分的测定。

关键词: 人参化妆品, 人参皂苷Rg1, 人参皂苷Re, 液质联用

Abstract:

A method was established for the determination of ginseng functional components （ginsenoside Rg1, ginsenoside Re） in ginseng cosmetics with ultra-high performance liquid chromatography triple quadrupole mass spectrometry （UPLC/MS-MS）. This method was used to monitor the risk of 28 batches of samples sold on the market. The samples were extracted by methanol ultrasonic method. The mobile phase was 0.05% formic acid aqueous solution - 0.05% formic acid acetonitrile solution, and the gradient elution was carried out. The samples were separated on the ACQUITY UPLC BEH C₁₈ （2.1 mm×100 mm×1.7 μm） column and detected by UPLC/MS-MS negative ion mode. At the same time, the pretreatment conditions and UPLC/MS-MS conditions were optimized and the method was verified. The results show that the method shows good linearity in the concentration range of 0.1-50 ng/mL and 0.5-200 ng/mL, with R² no less than 0.999 6. The limits of detection are in the range of 0.001 7-0.003 0 μg/g （S/N=3） . The average recoveries in sample matrix of cream, lotion and shampoo are from 81.87% to 94.45%, with relative standard deviations （RSDs） less than 5.64 （n=6） . This method is suitable for the determination of ginseng functional components in ginseng cosmetics.

Key words: ginsen cosmetics, ginsenoside Rg1, ginsenoside Re, UPLC/MS-MS

中图分类号:

TQ658

张伟清,侯俐南,李彬,刘慧锦,王海燕. 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.

ZHANG Wei-qing,HOU Li-nan,LI Bin,LIU Hui-jin,WANG Hai-yan. Determination of ginseng functional components in ginseng cosmetics by UPLC/MS-MS[J]. China Surfactant Detergent & Cosmetics, 2021, 51(6): 577-582.

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参考文献 17

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化合物名称	前体离子	产物离子	Q1 Pre Bais/V	CE/V	Q3 Pre Bais/V
Rg1	845.5	799.4^*	-24	-27	-22
Rg1	845.5	637.4	-24	-35	-40
Re	945.5	799.4^*	-22	-45	-16
Re	945.5	637.4	-22	-45	-20

成分	线性范围/（ng·mL^-1）	标准曲线	R²	LOQ/（μg·g^-1）	LOD/（μg·g^-1）
Rg1	0.1~50	y=39 611x+5 231	0.999 9	0.006 7	0.001 7
Re	0.5~200	y=1 319x+762	0.999 6	0.110 0	0.030 0

成分	添加浓度/（μg·g^-1）	膏霜类		乳液类		洗护类
成分	添加浓度/（μg·g^-1）	回收率/%	RSD/%	回收率/%	RSD/%	回收率/%	RSD/%
Rg1	0.5	94.13	4.74	86.97	3.40	81.95	3.52
	1.0	93.41	4.27	90.00	2.64	83.76	2.31
	2.0	94.45	5.64	88.87	4.08	81.87	2.51
Re	0.5	93.78	1.67	89.06	4.65	87.30	2.67
	1.0	92.22	3.47	87.52	2.91	86.35	2.97
	2.0	91.78	3.71	86.52	2.89	86.10	0.86

编号	产品名称	Rg1含量/（μg·g^-1）	Re含量/（μg·g^-1）
1	**牌密集强韧洗发水（油性头发）	3.39	6.83
2	**牌臻参焕活御时生机洗发水	0.07	0.17
3	**牌无硅油洗发露	未检出	未检出
4	**牌人参滋养修护发膜	0.01	检出,低于定量限
5	**牌控油祛痘洁面膏	未检出	未检出
6	**牌修护人参面膜	未检出	未检出
7	**牌人参维生素E乳	0.97	1.17
8	**牌补水舒缓面膜	未检出	未检出
9	**牌人参玉容养肤水	未检出	未检出
10	**牌人参矿物睡眠面膜	未检出	未检出
11	**牌人参修护调理液	3.19	7.30
12	**牌人参滋养修护洗发露	0.01	未检出
13	**牌SOD蛋白霜	0.25	0.59
14	**牌活力霜	0.04	0.11
15	**牌人参活肤精华霜	未检出	未检出
16	**牌SOD蜜	0.07	0.18
17	**牌人参滋养修护润发乳	未检出	未检出
18	**牌提拉紧致眼霜	0.04	0.10
19	**牌提拉紧致面霜	0.06	0.10
20	**牌赋活乳霜	检出,低于定量限	未检出
21	**牌倍润保湿霜	4.26	10.80
22	**牌人参嫩肤乳	未检出	未检出
23	**牌人参护发精华乳	未检出	未检出
24	**牌御容全能面霜	未检出	未检出
25	**牌御容精华水	未检出	未检出
26	**牌水光弹润精华乳	未检出	未检出
27	**牌轻透防晒隔离乳SPF30	未检出	未检出
28	**牌美白保湿霜	0.16	0.49