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

Abstract

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

CLC Number:

TQ658

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.

Figures/Tables 6

Tab. 1

Tab. 2

Fig. 1

Fig. 2

Tab. 3

Fig. 3

References 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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Study on the detection of preservatives in infant and adult skin care products by HPLC

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