市售无添加防腐剂化妆品防腐体系效能评价

doi:10.3969/j.issn.1001-1803.2021.10.008

摘要/Abstract

摘要：

通过中和剂验证、防腐挑战等试验对市售无添加防腐剂化妆品的防腐体系进行效能评价。采集无防腐剂的化妆品15批次,按《化妆品安全技术规范》（2015年版）（以下简称《规范》）进行菌落总数、霉菌和酵母菌以及pH值测定,参照GB 5009.238—2016《食品安全国家标准食品水分活度的测定》测定水活度,参考国外相关标准进行防腐挑战试验。菌落总数、霉菌和酵母菌的结果均符合《规范》要求。中和剂验证试验有3批（20%）需要替换中和剂或进一步稀释。防腐挑战试验中有14批细菌7天可下降大于99.9%,9批霉菌和酵母菌7天可下降大于90%。9批（60%）样品符合CTFA和AOAC非眼用化妆品的要求。样品普遍为弱酸性或中性,pH值最高9.73,最低4.68;水活度值集中在0.850~1.000,最低为0.643。综合结果表明：按《规范》进行化妆品微生物检验漏检风险较大,部分无添加防腐剂化妆品的防腐体系可能存在安全隐患;中和剂验证及防腐挑战试验亟需加入我国标准体系。

关键词: 化妆品, 无添加防腐剂, 防腐体系, 效能评价

Abstract:

The preservative performance of preservative-free cosmetics in the market was evaluated by neutralizer verification and preservative challenge testing. 15 batches of cosmetics without preservatives were collected. Total Aerobic Microbial Count （TAMC）, Total Molds and Yeasts Count （TMYC） and pH value were determined according to “Safety and Technical Standards for Cosmetics” （2015 Edition）（hereinafter referred to as the Standards）. Water activity was determined according to GB 5009.238—2016 “National Food Safety Standard Determination of Water Activity of Food”. Preservative challenge testing was carried out according to the methods of relevant foreign standards. The results of TAMC and TMYC meet the requirements of the Standards. The results of neutralizer verification show that 3 batches （20%） need neutralizer to be replaced or further diluted. The results of preservative challenge testing show that, bacteria of 14 batches decrease by more than 99.9% in 7 days, and molds and yeasts of 9 batches decrease by more than 90% in 7 days. Only 9 batches （60%） of the samples meet the requirements of non-eye cosmetics of CTFA and AOAC. Samples are generally weakly acidic or neutral, with the highest pH value of 9.73 and the lowest of 4.68. The water activity of most samples is in the range of 0.850-1.000, except for the ones with the low values of 0.643 and 0.751. It is shown that, in microbiological determination, the risk of missing rate will be high according to the methods of the Standards, and some preservative-free cosmetics may have potential safety hazards; it is urgent to introduce the neutralizer verification and preservative challenge testing to the national standards of microbiological test for cosmetics.

Key words: cosmetics, preservative-free, preservation, efficiency evaluation

中图分类号:

TQ658

李增婷,吕鑫,李倩,曹乾超,崔学文. 市售无添加防腐剂化妆品防腐体系效能评价[J]. 日用化学工业, 2021, 51(10): 975-980.

Li Zengting,Lyu Xin,Li Qian,Cao Qianchao,Cui Xuewen. Evaluation of preservation for preservative-free cosmetics[J]. China Surfactant Detergent & Cosmetics, 2021, 51(10): 975-980.

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参考文献 17

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编号	剂型	规格	批号	生产日期（保质期）/限期使用日期	原产国	可作为无添加防腐剂的成分
1	乳液	15 mL	54S601	202206	中国	丙二醇
2	乳液	50 mL	J0709A13	20220728	中国	丙二醇、丁二醇、戊二醇、己二醇、乙基己基甘油
3	面霜	45 g	H1011F18	20211021	中国	丙二醇、丁二醇、戊二醇、己二醇、乙基己基甘油
4	洗面霜	100 g	N0002979	20241023	日本	丁二醇、多种植物提取物
5	面霜	15 g	Y200511J1S	20230510	中国	丁二醇、戊二醇
6	精华	30 mL	Y200401S1J	20230331	中国	丁二醇、戊二醇
7	洁面乳	95 g	1M12GT11	20230211	中国	丁二醇、多种植物提取物
8	精华	30 mL	YEE130502	20200511（9个月）	中国	丁二醇、多种植物提取物、多种微生物发酵产物
9	水	180 mL	ID004	20211029	韩国	丙二醇、丁二醇、戊二醇、己二醇、多种植物提取物
10	水	80 mL	201903211H2Y	20220321	中国	己二醇、多种植物提取物
11	面霜	50 g	Y200521J15	20230520	中国	丁二醇、戊二醇、多种植物提取物
12	面霜	50 g	ARL11	20220510	中国	丁二醇、戊二醇、己二醇、辛酸甘油三酯、对羟基乙酮
13	精华	30 mL	KY200603	20220602	中国	多种植物提取物
14	水	180 mL	14ACF1C	20210313	日本	丁二醇、戊二醇
15	水	200 mL	AV675	202205	法国	水杨酸（标签中标注为皮肤调理剂,但其本身也是防腐剂）

编号	回收比值
编号	GP	GN	YM
1	0.75	0.58	1.16
2	0.87	1.20	1.26
3	1.44	1.22	1.03
4	0.21	1.40	0.40
5	1.13	1.40	1.01
6	1.05	1.28	1.09
7	0.61	1.21	1.00
8	0.95	1.27	1.10
9	1.21	1.24	0.99
10	1.08	1.32	0.94
11	1.40	1.39	1.03
12	1.13	1.20	0.94
13	0.94	1.41	1.01
14	1.08	0.80	1.04
15	1.02	1.19	1.17

编号	降低率/%
编号	1 d	7 d	14 d	28 d
1	100.0	100.0	100.0	100.0
2	100.0	100.0	100.0	100.0
3	100.0	100.0	100.0	100.0
4	100.0	100.0	100.0	100.0
5	100.0	100.0	100.0	100.0
6	100.0	100.0	100.0	100.0
7	100.0	100.0	100.0	100.0
8	63.4	100.0	100.0	100.0
9	99.9	100.0	100.0	100.0
10	99.8	100.0	100.0	100.0
11	100.0	100.0	100.0	100.0
12	99.8	100.0	100.0	100.0
13	99.7	100.0	100.0	100.0
14	64.3	99.8	100.0	100.0
15	100.0	100.0	100.0	100.0

编号	降低率/%
编号	1 d	7 d	14 d	28 d
1	84.4	100.0	100.0	100.0
2	60.4	93.9	100.0	100.0
3	69.8	96.7	100.0	100.0
4	41.7	59.4	87.0	98.6
5	87.5	63.5	62.5	82.3
6	65.6	75.0	69.8	76.0
7	79.2	97.9	100.0	100.0
8	25.0	100.0	100.0	100.0
9	63.5	88.5	98.9	100.0
10	91.0	100.0	100.0	100.0
11	37.5	78.1	75.0	79.2
12	25.0	100.0	100.0	100.0
13	65.6	100.0	100.0	100.0
14	56.3	71.9	64.6	76.0
15	88.5	100.0	100.0	100.0

编号	pH值	水活度
1	5.60	0.896
2	5.92	0.888
3	6.30	0.972
4	6.64	0.643
5	5.96	0.975
6	6.02	0.975
7	9.73	0.751
8	7.25	0.959
9	6.30	0.956
10	4.68	0.979
11	5.89	0.898
12	5.87	0.899
13	6.62	0.896
14	7.87	0.958
15	5.00	0.893
平均	6.38	0.903