归芩牙膏中阿魏酸、黄芩苷含量测定及其药效学研究

doi:10.3969/j.issn.2097-2806.2023.11.015

Abstract

Abstract:

A method for determining the content of ferulic acid and baicalein in the toothpaste by high performance liquid chromatography （HPLC） was established, and its pharmacological effects such as anti-inflammatory, analgesic and hemostatic effects were studied. Angelica and Baical skullcap root are the main medicines of Gui Qin toothpaste. The content of ferulic acid and baicalein, the main components of Gui Qin toothpaste, was determined by HPLC. The column was Agilent ZOBAX SB C₁₈ （2.1 mm×150 mm, 5 μm）, the mobile phase was acetonitrile-0.2% acetic acid aqueous solution （gradient elutation）, the flow rate was 1.0 mL/min, the detection wavelength was 320 nm, and the column temperature was 35 ℃. The anti-inflammatory, analgesic and hemostatic effects of Gui Qin toothpaste were investigated by establishing a model of xylene-induced ear swelling, mouse hot plate method and mouse liver wound bleeding model. The expression of inflammatory factors such as tumor necrosis factor-α （TNF-α）, interleukin-1β （IL-1β） and interleukin-6 （IL-6） in the mouse ear tissues was detected by ELISA. The injection rates of ferulic acid and baicalin show a good linear relationship between the injection concentration and the peak area in the range of 3.04-304 μg/mL and 2.86-286 μg/mL, respectively （R²>0.999 7）. The RSDs of the precision, stability and repeatability tests are less than 3.0%. The average dosing recovery rates are 98.95% and 99.87%, and the RSDs are 1.51% and 0.22%, respectively. The sample should contain no less than 0.54 mg of ferulic acid per 1 g and no less than 16.8 mg of baicalin. The HPLC method has strong specificity, good repeatability and stability, and can be used for quality control of Gui Qin toothpaste. Pharmacodynamic experiments have shown that Gui Qin toothpaste has good anti-inflammatory, analgesic and hemostatic effects. This study provides an experimental basis for the development and clinical application of Gui Qin toothpaste in the later stage.

Key words: Gui Qin toothpaste, ferulic acid, baicalein, content determination, high performance liquid chromatography

CLC Number:

TQ658

Zheng Lixia, Gao Huiqin, Li Sa, Guo Congjia, Hao Qianying, Wu Guotai. Determination of ferulic acid and baicalin content in Gui Qin toothpaste and its pharmacodynamic study[J].China Surfactant Detergent & Cosmetics, 2023, 53(11): 1345-1350.

Figures/Tables 13

Tab. 1

Fig. 1

Fig. 2

Fig. 3

Tab. 2

Tab. 3

Tab. 4

Tab. 5

Tab. 6

Tab. 7

Tab. 8

Tab. 9

Tab. 10

References 11

[1]	National Pharmacopoeia Commission. Pharmacopoeia of the people’s republic of China Part I[M]. Beijing: China Medical Science and Technology Press, 2020: 139.
[2]	Ling Ying, Xi Xiaojuan, Liu Qiaoli, et al. Research progress on physiological activity and application of ferulic acid and its derivatives[J]. Journal of Food and Biotechnology, 2018, 37 (5) : 449-454.
[3]	Cao Yindong. Analysis of the chemical composition and pharmacological effects of angelica[J]. The World’s Latest Medical Information Digest, 2019, 19 (2) : 93-95.
[4]	Li Bo. Observation of the efficacy of periodontal pouch with built-in drugs on periodontal disease[J]. Chinese Medical Guide, 2015, 13 (18) : 189-190.
[5]	Ding Guanjun, Zhang Kai, Cheng Jiping, et al. Research progress of skullcap extract in oral care[J]. Oral Care Products Industry, 2016, 26 (5) : 8-13.
[6]	Yuan Jiadao, Zhao Fang, Li Gaotian, et al. One test and multiple evaluation method simultaneously determined 6 ingredients in peony soup[J]. Proprietary Chinese Medicines, 2021, 43 (11) : 2970-2975.
[7]	Zhagn Guiping, Yang Rongbo, Wang Pingsheng. HPLC-PDA method simultaneously determined the content of five components in Bengu granules[J]. Zhongnan Pharmacy, 2020, 18 (1) : 117-120.
[8]	Ou Kaixi, Liu Jie, Zhao Yvming, et al. Study on the anti-inflammatory and analgesic efficacy of Feng Heatclear oral liquid and its mechanism[J]. Chinese Journal of Basic Medicine of Traditional Chinese Medicine, 2021, 27 (7) : 1104-1107, 1110.
[9]	Huang Guangwei, Liang Xuesong, Huang Jing, et al. Pharmacological test of anti-inflammatory effect of traditional Chinese medicine toothpaste with forsythia and honeysuckle as the medicine[J]. Oral Care Products Industry, 2022, 32 (4) : 28-29.
[10]	Zhang Jingjie. Development of eucommia leaf health toothpaste[D]. Kaifeng: Henan University, 2020.
[11]	Qin Yi, Sun jiabin, Zhang Hongling, et al. The main pharmacodynamic study of Rehabilitative toothpaste[J]. Asia-Pacific Traditional Medicine, 2018, 14 (9) : 16-19.

时间/min	φ（流动相A）/%	φ（流动相B）/%
0~ 2	13	87
2~18	13→30	87→70
18~25	30	70
25~28	30→13	70→87
28~30	13	87

	线性方程	R²	线性范围/（μg/mL）
阿魏酸	Y=102.44X+94.545	0.999 7	3.04~304
黄芩苷	Y=41.778X-10.751	0.999 9	2.86~286

成分	样品含量/mg	加入量/mg	测得量/mg	加样回收率/%	平均加样回收率/%	RSD/%
阿魏酸	0.053 6	0.04	0.093 0	98.50	98.95	1.51
	0.054 0	0.04	0.092 6	96.50
	0.054 2	0.04	0.093 8	99.00
	0.052 4	0.05	0.102 8	100.80
	0.053 6	0.05	0.102 0	96.80
	0.054 2	0.05	0.104 0	99.60
	0.053 6	0.06	0.114 0	100.67
	0.052 4	0.06	0.112 0	99.33
	0.053 0	0.06	0.112 6	99.33
黄芩苷	1.685 6	1.34	3.026 0	100.03	99.87	0.22
	1.680 2	1.34	3.016 6	99.73
	1.690 6	1.34	3.022 0	99.36
	1.680 2	1.68	3.359 0	99.93
	1.690 6	1.68	3.369 0	99.91
	1.679 8	1.68	3.360 2	100.02
	1.680 2	2.01	3.686 0	99.79
	1.681 4	2.01	3.690 0	99.93
	1.685 6	2.01	3.697 4	100.09

成分	阿魏酸峰面积/（mAU·min）	ρ（阿魏酸）/（μg/mL）	阿魏酸含量/%	黄芩苷峰面积/（mAU·min）	ρ（黄芩苷）/（μg/mL）	黄芩苷含量/%
1	847.6	7.35	0.054	9 480.9	227.19	1.68
2	847.0	7.35		9 479.6	227.16
3	846.4	7.34		9 479.5	227.16

组别	剂量	耳廓肿胀度	肿胀抑制率/%
空白组	0.2 mL NS	—	—
模型组	0.2 mL NS	8.25±1.80	—
阳性对照组	0.2 g	4.63±1.56^**Δ	43.94
牙膏基质组	0.2 g	6.09±0.92^*	26.21
归芩牙膏组	0.2 g	4.11±1.54^**ΔΔ	50.15

Determination of ferulic acid and baicalin content in Gui Qin toothpaste and its pharmacodynamic study

RichHTML

PDF (PC)

Like

Knowledge

Abstract

Cite this article

share this article

Figures/Tables 13

References 11

Related Articles 15

Metrics

Comments

Recommended 10

组别	剂量	ρ（TNF-α）/（ng/L）
空白组	0.2 mL NS	932.5 ±20.41
模型组	0.2 mL NS	1 178.85±37.83^**
阳性对照组	0.2 g	1 098.65±67.75
牙膏基质组	0.2 g	1 158.02±94.08
归芩牙膏组	0.2 g	1 068.96±48.32^ΔΔ

组别	剂量	ρ （IL-1β）/（ng/L）
空白组	0.2 mL NS	102.34±10.10
模型组	0.2 mL NS	164.95±16.95^**
阳性对照组	0.2 g	131.73±19.58^ΔΔ??
牙膏基质组	0.2 g	152.98±14.08^?
归芩牙膏组	0.2 g	107.18±12.23^ΔΔ????

组别	剂量	ρ（IL-6）/（pg/mL）
空白组	0.2 mL NS	124.04±18.29
模型组	0.2 mL NS	167.63±11.18^**
阳性对照组	0.2 g	144.39±14.74^ΔΔ?
牙膏基质组	0.2 g	160.42±14.59^?
归芩牙膏组	0.2 g	134.94±11.43^ΔΔ??

组别	剂量	给药前痛阈值/s	给药后不同时间痛阈值/s			痛阈值提高率/%
组别	剂量	给药前痛阈值/s	15 min	30 min	45 min	痛阈值提高率/%
空白组	0.2 mL NS	11.11±3.43	11.91±3.26	12.32±3.37	12.31±3.95	9.67
阳性对照组	0.2 g	11.50±2.16	16.31±1.61^**Δ	17.32±2.24^**Δ	18.27±2.54^**Δ	50.42
牙膏基质组	0.2 g	11.20±1.60	11.52±1.76	11.88±1.92	11.99±1.75	5.38
归芩牙膏组	0.2 g	11.88±3.30	16.62±4.25^*Δ	17.77±4.35^**Δ	18.44±4.67^**Δ	48.27

组别	剂量	止血时间/s	止血降低率/%
空白组	0.1 mL NS	72.84±9.23	—
阳性对照组	0.1 mL	33.79±6.88^**ΔΔ	53.61
牙膏基质组	0.1 mL	66.27±5.77	9.02
归芩牙膏组	0.1 mL	23.37±3.21^**ΔΔ	67.92

[1]	Liyuan Zhang, Linqi Yan, Qiaoyuan Cheng, Lvye Qi, Rong Wang, Liuqian Huang. Determination of 14 kinds of α-hydroxy acids and hydroxy esters in cosmetics [J]. China Surfactant Detergent & Cosmetics, 2024, 54(3): 353-359.
[2]	Hongling Zhang, Lin Cheng, Haiyan Wang, Feiya Luo, Huiliang Zhang, Lei Sun. Using DPRA alternative method to evaluate the skin sensitization of 3 coumarins [J]. China Surfactant Detergent & Cosmetics, 2024, 54(2): 156-160.
[3]	Huiduan Long, Yixiang Lu, Jianglan Qin, Keming Zhang. Simultaneous determination of 24 coumarin compounds in cosmetics by high performance liquid chromatography and verification by liquid chromatography-tandem mass spectrometry [J]. China Surfactant Detergent & Cosmetics, 2024, 54(1): 114-122.
[4]	Xue Xiao, Huirong Zhang, Shuowen Li, Sunhua Li, Miaomiao Guo, Li Li. Determination of four polyphenols and study on antioxidant and anti-inflammatory activities of extracts from callus of Eryngium maritimum L. [J]. China Surfactant Detergent & Cosmetics, 2024, 54(1): 57-64.
[5]	Xiong Jie, Yang Dan, Meng Hong, He Yifan, Pei Xiaojing. Research progress in skin physiological effects and its cosmetic encapsulation technology of ferulic acid [J]. China Surfactant Detergent & Cosmetics, 2023, 53(9): 1073-1079.
[6]	Feng Li,Zou Baisong. Simultaneous determination of 11 components in Danzhi Fangshaishuang SFP50 by HPLC [J]. China Surfactant Detergent & Cosmetics, 2023, 53(8): 968-975.
[7]	Wang Hongdan,Xu Weichang,Wang Yuan,Kong Xiangwen,Sun Lijuan. Determination of asiaticoside and madecassoside in Centella asiatica （L.） Urban by HPLC-ELSD [J]. China Surfactant Detergent & Cosmetics, 2023, 53(8): 976-980.
[8]	Liu Ying, Lin Min, Dai Sirui. Simultaneous determination of nine effective components in Polygonum Multif lorum Fangtuoyufa Jinghuaye by HPLC-QAMS [J]. China Surfactant Detergent & Cosmetics, 2023, 53(7): 841-848.
[9]	Yu Haiying, Qiao Zhenyun, Li Qiyan, Hu Defu, Niu Shuijiao, Wang Faping. Determination and isomer distribution of a cosmetic raw material hydroxypropyl tetrahydropyrantriol by HPLC [J]. China Surfactant Detergent & Cosmetics, 2023, 53(6): 721-724.
[10]	Gao Ruifang, Chai Ge, Li Xiangsheng. Determination of 47 kinds of dyestuffs in oxidative hair dye by high performance liquid chromatography [J]. China Surfactant Detergent & Cosmetics, 2023, 53(6): 725-732.
[11]	Wu Yuanyang, Zhang Liyuan, Wang Ren, He Tingting. Determination of 10 prohibited stines in 3 different matrixes of cosmetics by HPLC-MS/MS [J]. China Surfactant Detergent & Cosmetics, 2023, 53(4): 481-486.
[12]	Deng Mengjie, Yi Guobin, Lv Ran, Liu Yafeng, Ye Dawei, Chen Jiazhi. Ferulic acid nanoethosomes: preparation, characterization, and performance of skin penetration in vitro [J]. China Surfactant Detergent & Cosmetics, 2023, 53(11): 1285-1292.
[13]	Wu Xiaoyan, Song Faxiang. Determination of 13 chemical components in Koujie gargle by HPLC [J]. China Surfactant Detergent & Cosmetics, 2023, 53(10): 1233-1240.
[14]	Wang Lei, Wu Yue, Tian Dong. Determination of five benzotriazole UV absorbers in cosmetics by ultrasonic extraction and high performance liquid chromatography [J]. China Surfactant Detergent & Cosmetics, 2023, 53(1): 109-114.
[15]	He Liying, Jiang Fengbing. Determination of 27 sulfonamides in cosmetics by ultra-high performance liquid chromatography-tandem mass spectrometry [J]. China Surfactant Detergent & Cosmetics, 2023, 53(1): 100-108.