HPLC法检测婴幼儿与成人护肤品中防腐剂添加情况的研究

doi:10.3969/j.issn.1001-1803.2022.11.014

摘要/Abstract

摘要：

为了探究婴幼儿和成人护肤品中防腐剂添加情况，以期为婴幼儿和成人护肤品中防腐剂的安全监控与质量研究积累科学数据。以市售的140批护肤类产品为研究对象，基于国家药品监督管理局2021年第17号通告为检验依据对样品中防腐剂进行检测，将检测结果统计分析。结果表明：线性相关系数均大于等于0.9969，加标回收率为91%~104%，RSD小于5.0%。产自广东省和上海市的样本较多，未出现超限度情况，未检出禁用组分。苯氧乙醇和尼泊金酯类的甲丙酯使用频率较高；苯氧乙醇在婴幼儿护肤品中使用率较高；甲丙酯均在驻留类产品中普遍复合添加，且成人护肤品中的使用率高。婴幼儿护肤品中单批样品检出1~3种组分最多共有54批，成人护肤品中单批样品检出1~3种组分最多共有62批。婴幼儿护肤品防腐剂使用量0~2.3%明显高于成人护肤品使用量。结论：该试验下婴幼儿与成人护肤类产品中多以添加1~3种防腐剂成为防腐主流，且以苯氧乙醇和尼泊金酯类的甲丙酯为主要组分。

关键词: 婴幼儿, 成人, 护肤品, 驻留类产品, 淋洗类产品, 防腐剂, 合理性, 检验分析

Abstract:

The situation of addition of preservatives in infant and adult skin care products was studied, which is expected to accumulate scientific data for the safety monitoring and quality research of preservatives therein. 12 preservatives were detected for 140 batches of skin care products based on the method for 23 preservatives as shown in the “Technical Specification for Safety of Cosmetics “ （2015 edition）（Announcement No. 17 of 2021, National Medical Products Administration）. The test results were statistically analyzed. The results showed that, the linear correlation coefficients were all greater than or equal to 0.996 9, the recovery rate of standard addition was 91%-104%, and the RSD was less than 5.0%. There were many samples from Guangdong Province and Shanghai, and no over-limits or prohibited components were detected. Phenoxyethanol, methylparaben and propylparaben are more frequently used; phenoxyethanol is frequently used in infant skin care products; methylparaben and propylparaben are commonly compounded in retention products, and the frequency of use in adult skin care products is high; the mixture of methylchloroisothiazolinone, methylisothiazolinone, magnesium chloride and magnesium nitrate has only been added to rinse-off products. There are a maximum of 1-3 components in a single batch of infant skin care products of 54 batches, and a maximum of 1-3 components in a single batch of samples in adult skin care products of 62 batches. The amount of preservatives in infant skin care products （0-2.3%） is significantly higher than that of adult skin care products （0.000 16%-1.19%）. In this test, presence of 1-3 preservatives in infant and adult skin care products has become the mainstream, and phenoxyethanol, methylparaben and propylparaben are the main preservative components.

Key words: infants and young children, adults, skin care product, retention product, rinse-off product, preservative, rationality, inspection and analysis

中图分类号:

TQ658

刘慧,李莉,刘婷媛,徐勤科,孙莺,郭朝晖. HPLC法检测婴幼儿与成人护肤品中防腐剂添加情况的研究[J]. 日用化学工业（中英文）, 2022, 52(11): 1241-1247.

Liu Hui,Li Li,Liu Tingyuan,Xu Qinke,Sun Ying,Guo Zhaohui. Study on the detection of preservatives in infant and adult skin care products by HPLC[J]. China Surfactant Detergent & Cosmetics, 2022, 52(11): 1241-1247.

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参考文献 13

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时间/min	φ（A）/%	φ（B）/%
0	90	10
5.0	90	10
29.0	50	50
41.0	65	35
52.0	35	65
57.0	5	95
62.0	90	10
67.0	90	10

防腐剂	婴幼儿护肤品				成人护肤品
	婴幼儿淋洗类产品		婴幼儿驻留类产品		成人淋洗类产品		成人驻留类产品
	检出批数/批	检出使用率/%	检出批数/批	检出使用率/%	检出批数/批	检出使用率/%	检出批数/批	检出使用率/%
卡松	12	34.3	0	0	14	40.0	0	0
2-溴-2-硝基丙烷-1，3-二醇	0	0	2	5.7	0	0	0	0
甲基异噻唑啉酮	13	37.1	1	2.9	9	25.7	0	0
苯甲醇	7	20.0	1	2.9	1	2.9	0	0
苯氧乙醇	13	37.1	21	60.0	11	31.4	20	57.1
4-羟基苯甲酸甲酯	5	14.3	16	45.7	21	60.0	22	62.9
苯甲酸	12	34.3	3	8.6	6	17.1	2	5.7
4-羟基苯甲酸乙酯	0	0	4	11.4	1	2.9	1	2.9
4-羟基苯甲酸异丙酯	0	0	0	0	0	0	0	0
4-羟基苯甲酸丙酯	0	0	7	20.0	14	40.0	12	34.3
4-羟基苯甲酸异丁酯	0	0	0	0	0	0	0	0
4-羟基苯甲酸丁酯	0	0	0	0	0	0	0	0

防腐剂	限值/%	检出范围/%
防腐剂	限值/%	婴幼儿淋洗类产品	婴幼儿驻留类产品	成人淋洗类产品	成人驻留类产品
卡松	≤0.001 5（淋洗类产品，不能和甲基异噻唑啉酮同时使用）；不得添加（驻留类产品）	0.000 64~0.000 12	0	0.001 5~0.000 55	0
2-溴-2-硝基丙烷-1， 3-二醇	≤0.1	0	0.044~0.004 4	0	0
甲基异噻唑啉酮	≤0.01	0.006 8~0.000 054	0.002 6	0.008 2~0.000 16	0
苯甲醇	≤1.0	0.30~0.011	0.52	0.019	0
苯氧乙醇	≤1.0	0.88~0.21	0.77~0.10	0.44~0.000 72	0.59~0.081
4-羟基苯甲酸甲酯	总量≤0.5（以酸计）	0.13~0.000 73	0.19~0.005 3	0.19~0.000 81	0.30~0.002
苯甲酸	≤0.4（以酸计）	0.45~0.038	0.44~0.070	0.28~0.003 9	0.025~0.005 8
4-羟基苯甲酸乙酯	≤0.4（以酸计）	0	0.066	0.005 9	0.024
4-羟基苯甲酸丙酯	丙酯及其盐类之和不得超过0.14（以酸计）	0	0.11	0.079~0.04	0.14~0.039
4-羟基苯甲酸丁酯	丁酯及其盐类之和不得超过0.14（以酸计）	0	0	0	0

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