茴香酸在护肤品中溶解工艺的研究及其应用

doi:10.3969/j.issn.1001-1803.2021.10.010

Abstract

Abstract:

The antibacterial effect of anisic acid gradually highlights its advantages in non-preservative skin care products. However, its insoluble property in water greatly limits its use in cosmetics. Therefore, in the production process of cosmetics, the problem of realizing and accelerating the dissolution of anisic acid needs to be further solved. In this paper, the dissolution process and application of anisic acid in cosmetic were studied by the control variable method. The effects of the dosage of L-arginine, 1,2-hexanediol, and deionized water, their dissolution time and temperature on the dissolution process of anisic acid were investigated. The better quality ratios among the influencing factors were screened out. The anisic acid was applied as a preservative to a face cream and a lotion, and their stability and microbial challenges were tracked. The results show that the mass ratio range of anisic acid that can be completely dissolved is anisic acid:L-arginine:1,2-hexanediol:deionized water=1:（0-1.5）:（5-20）:（0.5-100）; and the optimal quality ratio range is 1:（0.8-1.5）:（5-20）:（0.5-2）, with the obtained solution relatively stable. The optimal dissolution temperature of anisic acid is 69-75 ℃. Under the condition of the mass ratio of L-arginine of 0~0.2, a face cream and a lotion were prepared respectively. Both products have passed 12-week stability test at -15, 25, 40 and 48 ℃. Microscopic images show that the size and distribution of the emulsion formed in the aqueous solution of the face cream and lotion cream at different temperatures for 12 weeks are uniform and have good long-term stability. The results of the microbial challenge test show that the cream can pass the level 1 preservative challenge, and the lotion can pass the level 3.

Key words: anisic acid, dissolution, process, preservative challenge

CLC Number:

TQ658

Zhao Xuehua. Study on the dissolution process of anisic acid and its application in cosmetic[J].China Surfactant Detergent & Cosmetics, 2021, 51(10): 990-996.

Figures/Tables 11

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References 11

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	方案1	方案2	方案3	方案4
茴香酸	1	1	1	1
L-精氨酸	0,0.2,0.4,0.6,0.8,1,1.5	0,0.2,0.4,0.6,0.8,1,1.5	1	1
1,2-己二醇	0	10	0,1,2.5,5,10,20	10
去离子水	100	100	100	0,0.5,2,10,100

防腐等级	第0天菌种Lg值		细菌浓度Lg差值
	第0天菌种Lg值		第7天		第14天		第21天		第28天
	细菌	真菌	细菌	真菌	细菌	真菌	细菌	真菌	细菌	真菌
1级	6	5	≥4	≥3	≥4	≥3	≥4	≥3	≥4	≥3
2级			≥3	≥2	≥4	≥3	≥3	≥2	≥4	≥3
3级			≥2	≥1	≥3	≥2	/	/	≥4	≥3
4级			≥2	≥1	≥2	≥1	≥3	≥1	≥3	≥2

L-精氨酸质量配比	最终温度/℃	溶解时间/s	茴香酸溶解性
0	85	1 362	不完全溶解
0.2	85	1 362	不完全溶解
0.4	85	1 362	不完全溶解
0.6	85	1 362	不完全溶解
0.8	85	1 362	不完全溶解
1	85	1 214	不完全溶解
1.5	85	957	不完全溶解

L-精氨酸质量配比	最终温度/℃	溶解时间/s	茴香酸溶解性	24 h内状态变化
0	81	1 406	完全溶解	随温度下降,逐渐析出
0.2	76.6	843	完全溶解	随温度下降,逐渐析出
0.4	74.7	739	完全溶解	随温度下降,逐渐析出
0.6	74.6	538	完全溶解	随温度下降,逐渐析出
0.8	72.1	428	完全溶解	温度下降至30 ℃时,底部少许析出
1	69.1	392	完全溶解	隔天有1-2个结晶析出
1.5	67.2	238	完全溶解	无析出

1,2-己二醇质量配比	最终温度/℃	溶解时间/s	茴香酸溶解性	24 h内状态变化
0	79.0	1 114	不完全溶解	茴香酸刚加入时,漂浮在溶液表面;随温度下降,逐渐析出
1	78.9	923	完全溶解	茴香酸刚加入时,分散在溶液中;当天少许析出
2.5	78.5	767	完全溶解	茴香酸刚加入时,分散在溶液中;当天少许析出
5	78.3	620	完全溶解	茴香酸刚加入时,沉在溶液底部;隔天少许析出
10	69.1	392	完全溶解	隔天有1~2个结晶析出
20	68.1	231	完全溶解	无析出

Study on the dissolution process of anisic acid and its application in cosmetic

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去离子水质量配比	最终温度/℃	溶解时间/s	茴香酸溶解性	24 h内状态变化
0	85	1 800	不完全溶解	已溶解的不再析出
0.5	73.5	1 682	完全溶解	澄清透明
2	72.8	572	完全溶解	澄清透明
10	71.3	147	完全溶解	澄清透明
100	69.1	392	完全溶解	隔天有1~2个结晶析出

	成分	w/%
A相	甲基硬酯酰基牛磺酸钠	0.1
A相	去离子水	20
B相	十六/十八烷基糖甙	1.5
	甘油	8
	三辛酸/癸酸甘油酯	3
	二甲基硅油	1
	十六/十八醇	3.5
	其它油脂类	6.79
C相	茴香酸	0.15
	L-精氨酸	0.01
	1,2-己二醇	1
	去离子水	0.3
	保湿剂	0.28
	EDTA二钠	0.05
	剩余去离子水	53.439
D相	增稠剂	0.8
E相	香精、添加物	0.081

	成分	w/%
A相	茴香酸	0.13
	L-精氨酸	0.000 1
	1,2-己二醇	1
	去离子水	0.2
	保湿剂	0.1
	EDTA二钠	0.05
	剩余去离子水	80.248 8
B相	聚氧乙烯（25）山嵛醇醚	0.5
	硬脂酸柠檬酸甘油酯	0.8
	三辛酸/癸酸甘油酯	2
	二甲基硅油	1.5
	甘油	8
	其它油脂类	4.950 1
C相	增稠剂	0.35
D相	香精、添加物	0.171

名称	0点	第4周				第8周				第12周
名称	0点	25 ℃	40 ℃	48 ℃	-15 ℃	25 ℃	40 ℃	48 ℃	-15 ℃	25 ℃	40 ℃	48 ℃	-15 ℃
结构	慕斯状膏霜	√	√	√	√	√	√	√	√	√	√	√	√
气味	特征气味	√	√	√	√	√	√	√	√	√	√	√	√
颜色	乳白色	√	√	√	√	√	√	√	√	√	√	√	√
pH	5.65（标准5.3~5.7）	5.53	5.51	5.52	5.51	5.55	5.53	5.54	5.52	5.56	5.54	5.53	5.53
黏度	10.30 Pa·s （标准6~300 Pa·s）	/	/	/	/	/	/	/	/	126.70	113.30	76.00	141.40

样品	初始菌种浓度/（CFU·g^-1）		第0天菌种浓度Lg值		菌种浓度Lg值								防腐挑战判定
	初始菌种浓度/（CFU·g^-1）		第0天菌种浓度Lg值		第7天		第14天		第21天		第28天
	细菌	真菌	细菌	真菌	细菌	真菌	细菌	真菌	细菌	真菌	细菌	真菌
面霜	0	0	/	/	1	0	1.30	0	0	0	0	1	通过
空白样	0	0	6.89	5.95	7.14	5.90	7.04	5.70	7.02	5.81	/	/
Lg差值	0	0	/	/	5.89	5.95	5.84	5.90	7.04	5.70	7.02	4.81
润肤乳	0	0	/	/	3.5	3.28	2.56	2.46	1.48	1.90	1	1	通过
空白样	0	0	6.82	5.81	/	/	/	/	/	/	/	/
Lg差值	0	0	/	/	3.32	2.53	4.26	3.35	5.34	3.91	5.82	4.81

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