化妆品中黄芪提取液的质量控制技术研究

doi:10.3969/j.issn.2097-2806.2024.12.015

摘要/Abstract

摘要：

选取黄芪提取液中指标成分毛蕊异黄酮苷，采用高效液相色谱-二极管阵列检测器法（HPLC-DAD）研究其含量测定方法；采用高效液相色谱-电雾式检测器法（HPLC-CAD），建立黄芪提取液的特征图谱；同时对其重金属含量水平进行测定，建立黄芪提取液的质量控制技术。结果表明，在4~80 μg/mL测定质量浓度范围内毛蕊异黄酮苷峰面积与质量浓度的线性关系良好（r=0.999），相对标准偏差RSD=2.4%，加标回收率在99.2%~102.7%之间。黄芪提取液的特征图谱标定了14个共有峰，指认了其中5个共有峰，相似度在0.485~0.995之间。重金属铅、汞、镉的含量均小于检出限，砷的含量小于2 mg/kg。该方法结合定性与定量评价，操作简便，具有良好重复性及稳定性，能较全面控制黄芪提取液内在质量。可作为黄芪提取液的工艺优化依据和质量控制技术，并对其他以中药材提取液作为原料的化妆品的质量技术研究提供参考。

关键词: 黄芪提取液, 质量控制技术, 毛蕊异黄酮苷, 特征图谱, 重金属

Abstract:

Calycosin-7-glucoside, which is the target ingredient of the Astragalus membranaceus extraction solution, was studied by the high-performance liquid chromatography-diode array detector method （HPLC-DAD）, and a high-performance liquid chromatography-electrospray ionization detector method （HPLC-CAD） was also established for fingerprint chromatogram analysis. Meanwhile, the heavy metal content was tested to build a quality control standard for Astragalus membranaceus extraction solution. Result shows a good linearity in 4-80 μg/mL mass concentration range with the correlation coefficient r=0.999, RSD=2.4%, and the recovery rate is between 99.2%-102.7%. The fingerprint chromatogram analysis features with 14 specific peaks, including 5 identified components. The similarity is between 0.485 to 0.995. Content of heavy metals such as lead, mercury, and cadmium are below the detection limit, and the content of arsenic is less than 2 mg/kg. This research results can serve as process optimization basis and quality control standards for Astragalus membranaceus extraction solution, and provide reference to quality control and research guideline for other cosmetics using herbal extracts as raw materials.

Key words: Astragalus membranaceus extraction solution, quality control technology, calycosin-7-glucoside, fingerprint chromatogram, heavy metal

中图分类号:

TQ658

汪汝沛, 楚亮, 陈清影, 李文莉, 李春艳, 傅萍. 化妆品中黄芪提取液的质量控制技术研究[J]. 日用化学工业（中英文）, 2024, 54(12): 1524-1531.

Rupei Wang, Liang Chu, Qingying Chen, Wenli Li, Chunyan Li, Ping Fu. Research on the quality control technology for the Astragalus membranaceus extraction solution in cosmetics[J]. China Surfactant Detergent & Cosmetics, 2024, 54(12): 1524-1531.

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No.	Batch	Production date	Extracting solvent	Character
1	22022801	2022.02	V（MeOH）∶V（H₂O）=1∶1	Brown liquid
2	22022802	2022.02	V（MeOH）∶V（H₂O）=1∶1	Brown liquid
3	22022803	2022.02	V（MeOH）∶V（H₂O）=1∶1	Brown liquid
4	22022804	2022.02	MeOH	Dark brown liquid
5	221007	2022.10	H₂O	Light brown liquid
6	221008	2022.10	H₂O	Light brown liquid
7	221009	2022.10	H₂O	Light brown liquid
8	221211	2022.12	V（MeOH）∶V（H₂O）=1∶1	Brown liquid
9	221212	2022.12	V（MeOH）∶V（H₂O）=1∶1	Brown liquid
10	221213	2022.12	MeOH	Dark brown liquid
11	230625	2023.06	H₂O^*	Light brown liquid
12	230629	2023.06	H₂O^*	Light brown liquid
13	230727	2023.07	H₂O^*	Light brown liquid

Name	Detection method	Limit index
Calycosin-7-glucoside	HPLC-DAD	≥700 μg/g
Specific chromatogram	HPLC-CAD	≥0.9 （Similarity）
Pb	AAS	≤10 mg/kg
As	AFS	≤2 mg/kg
Hg	Mercury analyzer method	≤1 mg/kg
Cd	AAS	≤5 mg/kg

Name	Linear range	Regression equation	r	LOD	LOQ
Calycosin-7-glucoside	4~80 μg/mL	y=51 668.398 4x-21 443.267 8	0.999	0.03 μg/mL	0.1 μg/mL
Pb	0~4 mg/L	y=0.022 70x+0.000 13	0.999 9	0.043 mg/L	0.14 mg/L
As	0~20 μg/L	y=0.552 31x+0.000 22	0.999	0.015 μg/L	0.05 μg/L
Hg	0~10 ng	y=326.081x+10.123	0.999	0.01 ng	0.03 ng
Cd	0~0.8 mg/L	y=-0.004 455 51x²+0.129 892 20x-0.001 449 89	0.999 9	2.7 μg/L	9 μg/L

Name	Recovery rate/%	Average recovery rate/%	RSD/%
Calycosin-7-glucoside	99.2，100.8，100.4	100.9	1.2
	101.2，100.1，99.4
	102.1，102.1，102.7
Pb	97.9，94.6，96.5，92.3，93.5，91.6	94.4	2.6
As	88.7，87.7，88.9，86.0，85.0，87.6	87.3	1.8
Hg	96.1，94.2，98.1，91.1，94.2，94.8	94.8	2.5
Cd	91.5，93.3，93.1，93.8，93.7，91.7	92.8	1.1

No.	Batch	Content results/（μg/g）			Relative deviation/%
No.	Batch	Sample 1	Sample 2	Average	Relative deviation/%
1	22022801	71.89	71.80	72	0.1
2	22022802	67.99	67.65	68	0.5
3	22022803	68.75	69.27	69	0.8
4	22022804	739.6	724.1	732	2.1
5	221017	12.68	12.95	13	2.1
6	221018	12.80	12.73	13	0.5
7	221019	27.38	27.60	27	0.8
8	221211	82.24	81.48	82	0.9
9	221212	88.52	89.31	89	0.9
10	221213	850.5	842.0	846	1.0