高效液相色谱法分析化妆品中苯扎氯铵及苄索氯铵

doi:10.3969/j.issn.1001-1803.2022.09.016

Abstract

Abstract:

A method for simultaneous determination of benzalkonium chloride and benzethonium chloride in cosmetics was established by high performance liquid chromatography. Different types of chromatographic columns and mobile phase conditions were screened. Finally, C₈ column was used to separate benzethonium chloride and three kinds of homologues of dimethyl benzyl ammonium chlorides calculated with benzalkonium chloride. Methanol : 0.1 mol/L ammonium acetate buffer solution （pH=5） was used as the mobile phase for isocratic elution. The results were simultaneously determined by DAD at the wavelength of 260 nm. Compared with the methods recommended in Technical Specification for Safety of Cosmetics （2015 edition）, the detection method of benzalkonium chloride and the detection method of lauralkonium chloride, benzethonium chloride and cetalkonium chloride were optimized and combined. A C₈ column with a wide range of use was selected to achieve the simultaneous separation of the four components. Benzalkonium chloride and benzethonium chloride have good linear relationship in a certain mass concentration range, and the correlation coefficients are greater than 0.999 9. The recoveries were 90%-110% with RSD of 0.3%-4.4% （n=9） at three mass concentration gradients of low, medium and high for four different types of matrixes. This method has the advantages of simple operation, short analysis time, good sensitivity and reproducibility, and can be used for the simultaneous determination of benzalkonium chloride and benzethonium chloride in cosmetics.

Key words: HPLC, cosmetics, preservative, benzalkonium chloride, benzethonium chloride

CLC Number:

TQ658

Wang Qilin,Han Xiaoping,Li Zhenbing,Tang Qikui. Analysis of benzalkonium chloride and benzethonium chloride in cosmetics by HPLC[J].China Surfactant Detergent & Cosmetics, 2022, 52(9): 1023-1058.

Figures/Tables 7

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Tab. 5

Fig. 2

References 8

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序号	名称	称样量/g	定容体积/mL	ρ/（mg/L）
1	劳拉氯铵	0.011 51	10	1 127.980 0
2	米他氯铵	0.010 83		1 066.755 0
3	西他氯铵	0.010 74		1 024.596 0
4	苄索氯铵	0.011 88		1 140.480 0

序号	ρ/（mg/L）
序号	名称	系列1	系列2	系列3	系列4	系列5	系列6
1	劳拉氯铵	5.639 9	11.279 8	28.199 5	56.399 0	84.598 5	112.798 0
2	米他氯铵	5.333 7	10.667 5	26.668 8	53.337 7	80.006 6	106.675 5
3	西他氯铵	5.122 9	10.245 9	25.614 9	51.229 8	76.844 7	102.459 6
4	苄索氯铵	5.702 4	11.404 8	28.512 0	57.024 0	85.536 0	114.048 0

序号	名称	线性回归方程	相关系数	线性范围/（mg/L）	LOQ/（mg/L）	LOD/（mg/L）
1	劳拉氯铵	y=1 123.69x+99.370 4	0.999 9	5.639 9~112.798 0	0.4	0.1
2	米他氯铵	y=900.229x+672.909	0.999 9	5.333 7~106.675 5	0.5	0.2
3	西他氯铵	y=909.764x+690.049	0.999 9	5.122 9~102.459 6	0.6	0.2
4	苄索氯铵	y=2 490.15x-526.249	0.999 9	5.702 4~114.048 0	0.5	0.2

序号	成分名称	理论加标质量浓度/（mg/L）	水基类		乳液类		膏霜类		沐浴露
序号	成分名称	理论加标质量浓度/（mg/L）	平均值/%	RSD/%	平均值/%	RSD/%	平均值/%	RSD/%	平均值/%	RSD/%
1	劳拉氯铵	11.279 8	102.3	1.9	99.0	0.4	92.7	2.6	98.2	2.1
		56.399 0	96.7	2.1	101.8	1.2	109.7	3.9	115.3	0.9
		112.798 0	100.4	3.2	93.6	2.7	97.9	1.4	95.7	1.2
2	米他氯铵	10.667 6	93.2	0.4	99.2	4.4	94.3	1.5	96.7	0.8
		53.337 8	108.7	2.6	102.1	3.6	98.2	2.1	98.2	1.3
		106.675 5	94.0	3.7	97.5	0.7	99.1	0.9	97.8	2.3
3	西他氯铵	10.246 0	104.1	4.3	95.1	2.3	104.8	3.5	104.3	1.7
		51.229 8	92.8	1.0	108.4	0.2	100.2	0.9	98.2	0.9
		102.459 6	100.3	1.3	97.9	4.1	99.6	1.1	106.3	2.4
4	苄索氯铵	11.404 8	109.3	0.6	92.5	0.8	102.1	2.6	94.9	1.5
		57.024 0	95.2	2.4	96.3	1.1	100.1	0.7	102.3	1.2
		114.048 0	99.1	0.3	98.1	1.7	98.9	0.3	90.5	0.3

序号	名称	标示成分	苯扎氯铵含量/%	标示含量/%
1	滴眼液1号	苯扎氯铵	0.007	0.01
2	滴眼液2号	苯扎氯铵	0.048	0.05

Analysis of benzalkonium chloride and benzethonium chloride in cosmetics by HPLC

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