Optimized Preparation and Application of Natural Film-Forming Agent Based on Mixture Design of Experiment

doi:10.19894/j.issn.1000-0518.240169

Chinese Journal of Applied Chemistry ›› 2024, Vol. 41 ›› Issue (12): 1721-1731.DOI: 10.19894/j.issn.1000-0518.240169

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Optimized Preparation and Application of Natural Film-Forming Agent Based on Mixture Design of Experiment

Lan-Lan ZENG, Ling-Ling LIU(), Hong-Bin HUANG, Shi-Bo HUANG, Li-Jun WEN, Ze-Pai LI

Guangzhou Cadlian Cosmetics Technology Co. ，Ltd. ，Guangzhou 510470，China

Received:2024-05-27 Accepted:2024-11-10 Published:2024-12-01 Online:2025-01-02
Contact: Ling-Ling LIU
About author:liull@carslan.com.cn

Abstract

Abstract:

Film forming agent is added to cosmetics to form a film on the skin surface to improve the skin sticking and makeup holding of base makeup products. Chemical film forming agent has some problems， such as skin feeling sticky， poor skin compatibility， poor biodegradability， and burden on skin caused by long-term use. In order to obtain a natural film-forming agent， the polysaccharides of Tremella fuciformis， Bletilla striata and peach gum were studied. The present study focuses on the extraction of natural polysaccharides from Tremella fuciformis， Bletilla striata and peach gum. The composition composed of three kinds of polysaccharide was optimized by mixture design with the film's tensile strength， elongation at break， and contact angle with artificial sweat and sebum. The optimal composition was figured out by the regression models built for each evaluation indexes and obtain natural film forming agent， followed by evaluating its efficacy on the human body. Results showed that the suitable composition of polysaccharides was as follows， when m（Tremella fuciformis）∶m（Bletilla striata）∶m（peach gum） is 0.2∶0.25∶0.55，the film exhibits a tensile strength of 3.18 MPa， elongation at break of 126.60%， and a contact angle of 86.03（°）. The verification test proved the predicted value was consistent with the actual value， indicating the regression models were valid. Simultaneously， human testing results indicate that incorporating a natural film-forming agent with a mass fraction of 0.15% into the liquid foundation matrix enhances skin stratum corneum hydration and imparts long-lasting cosmetic effects.

Key words: Film-forming, Agent natural source, Plant polysaccharide, Tremella fuciformis polysaccharide, Bletilla striata polysaccharide, Peach gum polysaccharide

CLC Number:

O629.1

Lan-Lan ZENG, Ling-Ling LIU, Hong-Bin HUANG, Shi-Bo HUANG, Li-Jun WEN, Ze-Pai LI. Optimized Preparation and Application of Natural Film-Forming Agent Based on Mixture Design of Experiment[J]. Chinese Journal of Applied Chemistry, 2024, 41(12): 1721-1731.

Figures/Tables 11

Table 1 Optimum extraction conditions of polysaccharides from three kinds of plants

Sample name	Liquid-solid ratio （mL∶g）	Extraction temperature/℃	Extraction time/h	Ultrasound time/min
Tremella fuciformis	50∶1	80	1	50
Bletilla striata	60∶1	50	2	60
Peach gum	80∶1	100	3	50

Fig.1 Mixing simplex grid design formula test point distribution

Table 2 Mixing experiment design and results

Test number	A w（Tremella fuciformis）/%	B w（Bletilla striata）/%	C w（Peach gum）/%	Y₁	Y₂	Y₃
Test number	A w（Tremella fuciformis）/%	B w（Bletilla striata）/%	C w（Peach gum）/%	TS/MPa	E/%	CA/（o）
1	100.00	0.00	0.00	1.55	165.00	58.78
2	75.00	25.00	0.00	3.38	206.09	73.81
3	75.00	0.00	25.00	1.66	133.74	75.00
4	50.00	50.00	0.00	3.27	191.48	72.98
5	50.00	25.00	25.00	3.51	125.00	78.49
6	50.00	0.00	50.00	1.61	125.92	87.66
7	25.00	75.00	0.00	2.63	121.43	62.20
8	25.00	50.00	25.00	3.54	101.00	76.56
9	25.00	25.00	50.00	3.32	115.32	86.17
10	25.00	0.00	75.00	1.40	156.84	92.06
11	0.00	100.00	0.00	0.53	0.00	45.42
12	0.00	75.00	25.00	2.07	86.04	61.21
13	0.00	50.00	50.00	2.79	153.26	73.41
14	0.00	25.00	75.00	2.32	197.34	85.50
15	0.00	0.00	100.00	0.71	223.53	87.92
16	33.30	33.30	33.30	3.69	105.56	84.81
17	66.70	16.70	16.70	3.01	140.43	81.55
18	16.70	66.70	16.70	3.12	93.05	63.11
19	16.70	16.70	66.70	2.58	142.11	90.07

Table 3 Summary of regression equation model of evaluation index evaluation index

Index	Types of models	Equation of regression	S	R²	$R A d j 2$	$R F c 2$
Y₁（TS）	Cube	Y₁=1.586 1A+0.485 1B+0.785 9C+9.713AB+1.8AC+8.501BC+13.88ABC	0.114 459	0.990 9	0.986 3	0.969 9
Y₂（E/%）	Cube	Y₂=167.11A-0.56B+221.68C+432.3AB-267.3AC+164.5BC-1 628.9ABC	2.695 48	0.998 1	0.997 2	0.994 0
Y₃（CA）	Square	Y₃=59.92A+43.28B+89.58C+84.28AB+50.99AC+30.91BC	2.459 08	0.972 6	0.962 0	0.925 2

Table 3 Summary of regression equation model of evaluation index evaluation index

Index	Types of models	Equation of regression	S	R²	$R A d j 2$	$R F c 2$
Y₁（TS）	Cube	Y₁=1.586 1A+0.485 1B+0.785 9C+9.713AB+1.8AC+8.501BC+13.88ABC	0.114 459	0.990 9	0.986 3	0.969 9
Y₂（E/%）	Cube	Y₂=167.11A-0.56B+221.68C+432.3AB-267.3AC+164.5BC-1 628.9ABC	2.695 48	0.998 1	0.997 2	0.994 0
Y₃（CA）	Square	Y₃=59.92A+43.28B+89.58C+84.28AB+50.99AC+30.91BC	2.459 08	0.972 6	0.962 0	0.925 2

Fig.2 Residual plot of film tensile strength （A）， film elongation at break （B） and film contact angle （C）

Table 4 Analysis of variance for the regression model

Source	df			Seq SS			Adj SS			Adj MS			F				p
Source	Y₁	Y₂	Y₃	Y₁	Y₂	Y₃	Y₁	Y₂	Y₃	Y₁	Y₂	Y₃	Y₁	Y₂	Y₃	Y₁	Y₂	Y₃
Regression	6	6	5	17.02	46 813.8	2 789.51	17.02	46 813.8	2 789.51	2.84	7 802.3	557.90	216.6	1 073.87	92.26	**	**	**
Linear	2	2	2	1.45	19 587.2	2 075.54	0.96	39 855.5	1 634.7	0.48	19 927.7	817.35	36.72	2 742.76	135.16	**	**	**
Quadratic	3	3	3	15.20	22 097.4	713.97	7.88	23 097.8	7 13.97	2.63	7 699.3	237.99	200.45	1 059.69	39.36	**	**	**
AB	1	1	1	7.48	8 381.6	461.25	5.52	10 936.7	553.09	5.52	10 936.7	553.09	421.41	1 505.28	91.46	**	**	**
AC	1	1	1	0.31	13 693.5	178.33	0.19	4 182	202.43	0.19	4182	202.43	14.48	575.59	33.48	**	**	**
BC	1	1	1	7.41	22.3	74.38	4.23	1 583.3	74.38	4.23	1 583.3	74.38	322.81	217.92	12.3	**	**	**
ABC	1	1	-	0.37	5 129.2	-	0.37	5 129.2	-	0.37	5 129.2	-	28.44	705.95	-	**	**	-
Residual error	12	12	13	0.16	87.2	78.61	0.16	87.2	78.61	0.01	7.3	6.047
Total	18	18	18	17.18	46 900.9	2 868.12

Fig.3 Mixed surface map （A， C， E） and mixed contour map （B， D， F） of the influence of the proportion of three polysaccharides on film tensile strength， film elongation at break and film contact angle

Fig.4 The response tracking diagram and response optimization diagram of the influence of the proportion of three polysaccharides on film tensile strength (A)， film elongation at break (B) and film contact angle (C)

Table 5 Statistical results of the mass fraction of water in stratum corneum

w（warer in stratum corneum）/%	Group	0 h	0.5 h	4 h	8 h
Average value	Control group	33.45	54.56	55.83	54.21
Average value	Experimental group	36.12	59.90	64.13	62.12
SE value	Control group	1.75	1.79	2.64	2.09
SE value	Experimental group	1.63	1.87	2.08	2.22
ΔDifference value	Control group	/	20.6	22.4	21.2
ΔDifference value	Experimental group	/	23.7	28.0	26.4
Rate of change/%	Control group	/	63.47	67.07	62.28
Rate of change/%	Experimental group	/	65.93	77.56	72.02
p（after use vs before use）	Control group	/	**	**	**
p（after use vs before use）	Experimental group	/	**	**	**
p（control group vs experimental group）		/	*	**	**

Table 6 Contact angle between artificial sweat and artificial sebum and liquid foundation film

Group	CA/（°）			p
Group	G1	G2	G3	p
Synthetic perspiration（ $x ˉ$ ±S）	73.71±0.70	81.95±0.55	84.28±0.20	**
Synthetic sebum（ $x ˉ$ ±S）	26.71±0.51	28.18±0.20	30.15±0.15	**

Table 6 Contact angle between artificial sweat and artificial sebum and liquid foundation film

Group	CA/（°）			p
Group	G1	G2	G3	p
Synthetic perspiration（ $x ˉ$ ±S）	73.71±0.70	81.95±0.55	84.28±0.20	**
Synthetic sebum（ $x ˉ$ ±S）	26.71±0.51	28.18±0.20	30.15±0.15	**

Table 7 Subjects self-rated feedback results

Evaluation time	Evaluation dimension	D/%		［（G2-G1）/G1］/%
Evaluation time	Evaluation dimension	Control group G1	Experimental group G2	［（G2-G1）/G1］/%
Apply makeup within 30 min	1	78.75	80	1.56
	2	76.25	80	4.69
	3	70	81.25	13.85
	4	68.75	75	8.33
	5	66.25	75	11.67
	6	67.5	75	10.00
8 h after applying makeup	7	67.5	71.25	5.26
	8	66.25	70	5.36
	9	65	67.5	3.70
	10	67.5	70	3.57

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Optimized Preparation and Application of Natural Film-Forming Agent Based on Mixture Design of Experiment

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