气相色谱法测定淋洗类化妆品中的硅氧烷类物质

doi:10.3969/j.issn.1001-1803.2021.07.016

摘要/Abstract

摘要：

建立了气相色谱法测定淋洗类化妆品中高关注硅氧烷类物质,包括八甲基环四硅氧烷（D4）、十甲基环五硅氧烷（D5）、十二甲基环六硅氧烷（D6）及类似物六甲基环三硅氧烷（D3）、十四甲基环七硅氧烷（D7）、十六甲基环八硅氧烷（D8）的检测方法。以正己烷为提取溶剂,经萃取、过滤后外标法定量。6种环状硅氧烷质量浓度与峰面积之间呈良好的线性关系（r >0.998）,检出限为0.002%,定量限为0.005%。不同样品基质分别加入6种环状硅氧烷的回收试验中,洗发水平均回收率为77.1%~104.2%,相对标准偏差0.5%~6.7%;护发素平均回收率为72.1%~106.9%,相对标准偏差0.3%~3.8%;剃须膏平均回收率为71.5%~112.6%,相对标准偏差0.9%~9.2%;沐浴乳平均回收率为73.3%~118.7%,相对标准偏差0.2%~7.7%;洁面乳平均回收率为74.8%~104.6%,相对标准偏差0.2%~4.8%。方法准确度好、操作简单,可用于淋洗类化妆品中硅氧烷类物质的测定。

关键词: 淋洗类化妆品, 甲基环硅氧烷, 气相色谱

Abstract:

A method of GC-FID was used for the analysis of D4, D5, D6 and their analogs D3, D7, D8 in cosmetics. The samples were extracted, filtered and analyzed by gas chromatography, and quantified by external standard method. The results show that there is a good linearity between the peak area and the concentration of six cyclic siloxane in the range of 5-200 mg/L with the r values higher than 0.998. The detection limits for six cyclic siloxane are 0.002%, and the limits of quantification are 0.005%. The average recoveries of six cyclic siloxane in shampoo,conditioner,shaving cream, bath gel and cleanser are 77.1%-104.2%, 72.1%-106.9%, 71.5%-112.6%, 73.3%-118.7%, and 74.8%-104.6%, respectively. The method is simple, efficient, sensitive and reliable, and is suitable for the general detection of six cyclic siloxane in various kinds of rinse-off cosmetics. It can provide technical support for the protection of the global environment and human health.

Key words: rinse-off cosmetics, methylcyclosiloxane, gas chromatography

中图分类号:

TQ658

温晓静,唐璜,赵苑余,陈江,胡东平,王国民. 气相色谱法测定淋洗类化妆品中的硅氧烷类物质[J]. 日用化学工业, 2021, 51(7): 691-696.

Wen Xiaojing,Tang Huang,Zhao Yuanyu,Chen Jiang,Hu Dongping,Wang Guomin. Determination of methylcyclosiloxane in rinse-off cosmetics by gas chromatography[J]. China Surfactant Detergent & Cosmetics, 2021, 51(7): 691-696.

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参考文献 8

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化合物	线性范围/（mg·L^-1）	线性方程	相关系数	以样品计质量分数/%
D3	5~200	y=0.708 6x+1.420	0.998 9	0.005~0.2
D4	5~200	y=0.763 6x+1.540	0.998 9	0.005~0.2
D5	5~200	y=0.749 1x+1.548	0.998 9	0.005~0.2
D6	5~200	y=0.725 2x+1.559	0.999 0	0.005~0.2
D7	5~200	y=0.772 5x+1.530	0.998 9	0.005~0.2
D8	5~200	y=0.617 3x+1.227	0.999 0	0.005~0.2

成分	添加量/%	洗发水		护发素		剃须膏		沐浴乳		洁面乳
成分	添加量/%	回收率/%	RSD/%	回收率/%	RSD/%	回收率/%	RSD/%	回收率/%	RSD/%	回收率/%	RSD/%
D3	0.005	77.1	0.5	74.6	3.8	72.4	3.6	73.3	0.2	74.8	4.8
	0.01	80.2	2.2	88.6	0.5	82.3	4.9	85.3	1.9	82.2	0.3
	0.1	92.8	5.5	104.4	0.3	103.4	7.5	107.4	0.9	90.6	0.2
D4	0.005	87.9	0.6	74.7	0.5	79.8	1.7	85.1	3.1	91.8	2.4
	0.01	83.2	6.7	90.6	1.4	88.7	2.4	93.9	4.5	98.2	1.4
	0.1	97.6	2.2	106.7	0.4	106.5	5.6	110.7	0.9	96.3	0.2
D5	0.005	96.1	2.4	72.3	1.9	71.5	2.3	86.9	7.7	95.7	0.3
	0.01	81.9	4.5	90.2	0.3	87.0	1.8	95.7	5.4	95.5	0.5
	0.1	100.8	5.3	106.9	0.4	96.5	1.4	118.7	0.2	93.1	0.3
D6	0.005	104.2	4.1	72.1	1.7	75.6	7.7	74.1	1.7	82.8	2.6
	0.01	83.3	5.7	90.7	2.2	90.6	1.7	86.8	3.4	89.6	1.4
	0.1	99.3	5.3	106.9	0.4	112.6	9.2	111.0	0.6	91.4	0.3
D7	0.005	83.2	2.1	72.6	2.0	75.8	2.3	85.8	5.9	90.9	2.6
	0.01	80.2	1.2	91.5	1.4	84.8	0.9	98.4	3.1	92.9	4.1
	0.1	95.1	5.5	103.3	0.4	105.4	8.9	108.9	0.8	92.6	0.2
D8	0.005	83.1	1.8	77.6	2.2	87.9	5.0	93.8	2.2	104.6	2.7
	0.01	80.2	2.2	91.9	3.4	95.2	1.9	88.4	4.8	100.2	1.9
	0.1	97.6	5.9	97.1	0.4	107.4	8.2	104.7	0.9	90.5	0.4

产品	数量/个	D4	D5	D6	D7	D8
洁面产品	4	均未检出	1个检出,0.002 8%	均未检出	1个检出,0.002 0%	1个检出,0.007 4%
洗发产品	12	8个检出, 0.003 2%~0.018 9%	3个检出, 0.004 1%~0.007 7%	2个检出, 0.004 5%和0.004 8%	2个检出, 0.004 2%和0.002 5%	5个检出, 0.002 8%~0.010 5%
护发产品	9	4个检出, 0.002 1%~0.013 9%	3个检出, 0.002 2%~0.987 6%	4个检出, 0.002 9%~0.023 1%	4个检出, 0.0021%~0.0141%	2个检出, 0.014 1%和0.005 7%

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