高效液相色谱法同时检测染发类化妆品中5种限用染料

doi:10.3969/j.issn.1001-1803.2022.01.016

摘要/Abstract

摘要：

建立了染发类化妆品中1-羟乙基-4,5-二氨基吡唑硫酸盐等5种限用染料含量检测的高效液相色谱分析方法。样品经提取,过滤后,采用Agilent ZORBAX SB-C₁₈色谱柱（250 mm×4.6 mm,5 μm）分离,以甲醇为流动相A,5 mmol/L乙酸铵溶液为流动相B,梯度洗脱,流速为1.0 mL/min,柱温为30 ℃,二极管阵列检测器检测,标准曲线法定量。结果表明,5种限用染料的线性相关系数均大于0.999,低、中、高3种加标水平下5种限用染料的平均回收率为92.5%~106.0%,相对标准偏差为0.5%~4.1%。

关键词: 限用染料, 化妆品, 高效液相色谱法

Abstract:

A high performance liquid chromatography （HPLC） method for the determination of 5 restricted dyes in hair dyeing cosmetics was established. The sample was extracted and filtered, separated by an Agilent ZORBAX SB-C₁₈ column （250 mm×4.6 mm, 5 μm）, and gradient elution with methanol as mobile phase A and 5 mmol/L ammonium acetate solution as mobile phase B. The elution was performed at a flow rate of 1.0 mL/min and the column temperature was set at 30 ℃. The analysis was done using photo-diode array detector. Standard curve method was used for quantification. The results show that the linear correlation coefficients of the five restricted dyes are all greater than 0.999. The average recoveries at three spiked levels of the five restricted dyes are in the range of 92.5%-106.0% with RSDs of 0.5%-4.1%.

Key words: restricted dyes, cosmetics, high performance liquid chromatography

中图分类号:

TQ658

杨淡梅,石兴红,罗金梅,符秋美,邱颖姮,邬晓鸥,王晓炜. 高效液相色谱法同时检测染发类化妆品中5种限用染料[J]. 日用化学工业, 2022, 52(1): 103-108.

Yang Danmei,Shi Xinghong,Luo Jinmei,Fu Qiumei,Qiu Yingheng,Wu Xiaoou,Wang Xiaowei. Simultaneous determination of 5 restricted dyes in hair dyeing cosmetics by high performance liquid chromatography[J]. China Surfactant Detergent & Cosmetics, 2022, 52(1): 103-108.

图/表 5

表 1

表 2

图 1

表 3

表 4

参考文献 16

[1]	Dai Ming. Simultaneous determination of nine kinds of dyestuff in hair dyes by ultra performance liquid chromatography-tandem mass spectrometry[J]. China Surfactant Detergent & Cosmetics, 2017, 47(5) : 297-300.
[2]	Yang Yanwei, Liu Siran, Zhang Zhuona. Investigation of hair dyes in hair-dyeing cosmetics[J]. Chinses Journal Health Laboratory Technology, 2017, 27(6) : 899-901.
[3]	Compiled by Cosmetics Standard Expert Committee of State Food and Drug Administration. Safety and technical standards for cosmetics[M]. Beijing: People’s Health Press, 2016: 120-126, 409-415.
[4]	Kohd, Tanc, Ansk, et al. Screening for p-phenylenediamine (PPD) in hair-care products by thin-layer chromatography (TLC)[J]. Contact Dermatitis, 2000, 43:182-183. pmid: 10985645
[5]	Lu Xiaorui, Du Hongmiao, Zhang Zhe, et al. Determination of 20 kinds of banned and restricted dyestuffs in hair dyes by high performance liquid chromatography[J]. Detergent & Cosmetics, 2015, 38(12) : 31-34.
[6]	Chen Juan, Wang Chao, Wang Xing, et al. Simultaneous determination of nine dyestuffs and dyes intermediates in cosmetics by high performance liquid chromatography/photodiode array detection[J]. Chinese Journal of Chromatography, 2007, 25(6) : 867-870. pmid: 18257307
[7]	Zhang Guocui, Lu Yichuan, Li Chunling, et al. Simultaneous determination of 26 dyes in hair colorants by high performance liquid chromatography[J]. Flavour Fragrance Cosmetics, 2019, 10(5) : 43-47.
[8]	Li Hongying, Huang Cheng, Ding Xiaoping, et al. Determination of 21 kinds of banned and restricted dyestuffs in hair dyes by high performance liquid chromatography[J]. Flavour Fragrance Cosmetics, 2019, 8(4) : 28-32.
[9]	Zhu Weixia, Wang Caijuan, Yang Jizhou, et al. Simultaneous determination of 11 aminophenols in hair dyes by high performance liquid chromatography[J]. Chinese Journal of Chromatography, 2012, 30(9) : 870-875. pmid: 23285966
[10]	Chen Weiguang. Determination of phenylenediamine in oxidative-type hair dyes by capillary column gas chromatography[J]. Journal of Environment and Health, 2007, 24(4) : 258-260.
[11]	Lai Ying, Chen Hexiu, Lin Rui, et al. Simultaneous determination of 17 components in oxidative hair dyes by gas chromatography-mass spectrometry[J]. Chemical Journal of Chinese Universities, 2011, 32(10) : 2286-2292.
[12]	Ju Lingyan, Li Zhaojie, Song Weide, et al. Rapid screening of 32 dyes in oxidative hair dyes by ultra-performance liquid chromatography-quadrupole/electrostatic field obitrap high-resolution mass spectrometry[J]. Journal of Instrumental Analysis, 2019, 38(8) : 931-938.
[13]	Chen Meng, Hu Lei, Xu Li, et al. Simultaneous determination of 33 kinds of banned and/or restricted component in hair dyes by high performance liquid chromatography-mass spectrometry[J]. China Surfactant Detergent & Cosmetics, 2016, 46(6) : 359-364.
[14]	Lu Yuchao, Wang Haiyan, Song Pingping, et al. Determination of seven aromatic amines in hair dyes by capillary electrophoresis coupled with field-amplified sample stacking[J]. Chinese Journal of Chromatography, 2011, 29(11) : 1122-1127. pmid: 22393703
[15]	Li Xianqing, Wang Lingling. Simultaneous determination of eight dyes in oxidation hair dyes by high performance liquid chromatography[J]. Flavour Fragrance Cosmetics, 2013, 10(5) : 46-49.
[16]	Yan Wei, Hu Lei, Zhou Minghao. Determination of 32 kinds of banned and/or restricted dyestuff in hair dyes by high performance liquid chromatography[J]. China Surfactant Detergent & Cosmetics, 2015, 45(1) : 49-54.

	组分	标准溶液含量/%			样品溶液含量/%
	组分	2 h	5 h	10 h	2 h	5 h	10 h
未添加抗氧化剂	2-氨基-4-羟乙氨基茴香醚硫酸盐	86	75	67	79	24	19
未添加抗氧化剂	1,3-双-（2,4二氨基苯氨基）丙烷盐酸盐	84	78	76	92	56	58
添加亚硫酸氢钠	2-氨基-4-羟乙氨基茴香醚硫酸盐	99	97	94	99	95	91
添加亚硫酸氢钠	1,3-双-（2,4二氨基苯氨基）丙烷盐酸盐	99	98	98	99	98	97

组分	线性方程	线性范围/（mg/L）	相关系数	LODs/（mg/kg）
1-羟乙基-4,5-二氨基吡唑硫酸盐	y=1.076×10⁴ x-313.7	2.063~103.1	0.999 9	7.3
羟苯并吗啉	y=1.818×10⁴ x+352.1	0.441~110.2	0.999 9	1.9
2-氨基-4-羟乙氨基茴香醚硫酸盐	y=1.553×10⁴ x-422.1	0.475~118.9	0.999 9	2.4
2-甲基-5-羟乙氨基苯酚	y=2.389×10⁴ x+599.3	0.435~108.8	0.999 9	1.3
1,3-双-（2,4二氨基苯氨基）丙烷盐酸盐	y=1.800×10⁴ x-360.8	0.452~112.9	0.999 9	2.0

组分	添加水平/ （mg/L）	蜡质		膏霜		喷雾
组分	添加水平/ （mg/L）	回收率/%	RSD/%	回收率/%	RSD/%	回收率/%	RSD/%
1-羟乙基-4,5-二氨基吡唑硫酸盐	3.132 15.73 75.06	102.4 99.4 99.8	1.2 3.3 2.5	97.5 95.8 103.1	3.2 2.9 1.0	93.3 98.0 100.8	2.9 1.5 1.5
羟苯并吗啉	0.767 11.83 72.40	101.4 103.9 100.4	1.4 0.6 1.8	95.3 97.0 98.8	2.7 2.9 0.5	103.8 104.3 101.0	3.6 2.2 0.9
2-氨基-4-羟乙氨基茴香醚硫酸盐	0.809 11.54 73.38	101.9 103.2 99.4	1.3 1.3 3.1	99.3 102.8 104.4	1.3 1.5 0.6	96.2 103.7 102.2	2.1 1.1 1.2
2-甲基-5-羟乙氨基苯酚	0.646 10.48 76.41	102.4 103.9 101.2	1.9 0.6 1.6	98.1 92.7 100.0	1.9 2.6 0.5	95.8 106.0 101.8	3.6 0.5 0.5
1,3-双-（2,4二氨基苯氨基）丙烷盐酸盐	0.654 11.03 73.11	102.8 101.4 101.4	1.5 3.3 1.8	100.9 100.0 101.4	2.8 2.9 0.7	92.5 96.2 101.7	4.1 0.6 0.9

组分	含量/%
组分	样品1	样品2	样品3	样品4	样品5
1-羟乙基-4,5-二氨基吡唑硫酸盐	0.66	未检出	未检出	未检出	未检出
羟苯并吗啉	未检出	0.020	未检出	未检出	未检出
2-氨基-4-羟乙氨基茴香醚硫酸盐	未检出	未检出	未检出	未检出	0.004 5
2-甲基-5-羟乙氨基苯酚	未检出	未检出	未检出	0.069	未检出
1,3-双-（2,4二氨基苯氨基）丙烷盐酸盐	未检出	未检出	0.16	未检出	未检出