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

Abstract

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

CLC Number:

TQ658

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.

Figures/Tables 10

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References 23

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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

Research on the quality control technology for the Astragalus membranaceus extraction solution in cosmetics

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No.	Batch	Similarity	No.	Batch	Similarity
1	22022801	0.992	8	221211	0.993
2	22022802	0.982	9	221212	0.995
3	22022803	0.994	10	221213	0.991
4	22022804	0.991	11	230625	0.485
5	221007	0.933	12	230629	0.488
6	221008	0.936	13	230727	0.861
7	221009	0.928

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