高效液相色谱法同时测定祛痘类化妆品中的10种抗痤疮类化学成分及质谱确证

doi:10.3969/j.issn.1001-1803.2022.10.016

摘要/Abstract

摘要：

建立了同时检测祛痘类化妆品中的10种抗痤疮类成分（过氧苯甲酰、螺内酯、他卡西醇、他扎罗汀、阿维A、异维甲酸、维甲酸、依曲替酯、维胺酯、阿达帕林）的高效液相色谱-紫外筛查、定量方法及液相色谱-质谱定性确证方法。样品经甲醇提取后,经Agilent ZORBAX Extend-C18（4.6×250 mm,5 μm）色谱柱分离,以甲醇和乙酸水溶液为流动相梯度洗脱,PDA检测器多波长检测,外标法定量。结果表明,方法的回收率为80.8%~102.7%,相对标准偏差小于3.0%,10种抗痤疮类成分在各自的质量浓度范围内均呈良好的线性关系（相关系数均≥0.999 8）,检出限为0.1~1.0 mg/kg。该方法具有前处理步骤简单、分析时间短、准确性好等特点,适用于化妆品中祛痘类化妆品中的10种抗痤疮类成分的定性筛查及含量测定。

关键词: 高效液相色谱法, 液相色谱-串联质谱法, 祛痘类化妆品, 抗痤疮

Abstract:

The purpose was to establish a method for the identification of ten anti-acne compounds （benzoyl peroxide, spironolactone, tacalcitol, tazarotene, acitretin, isotretinoin, tretino-in, etretinate, viaminate, adapalene） in anti-acne cosmetics by high performance liquid chromatography and verification by liquid chromatography-tandem mass spectrometry. The samples were extracted by ultrasonic machine with methanol. The separation was executed on an Agilent ZORBAX Extend-C18 column by a mobile phase consisting of 0.5% acetic acid （A）, methanol （B）, with the flow speed of 1.0 mL/min. The qualitative screening results were obtained through high performance liquid chromatography with PDA detector at multi-wavelength, the standard curve method was used for quantification, and the results of liquid chromatography tandem mass spectrometry were used for verification. The results show that under the conditions of this method, the recovery rate is 80.8%-102.7%, and the relative standard deviation is less than 3.0%. Ten anti-acne compounds obtain a good linear relationship within their respective mass concentration ranges, and the correlation coefficients are all greater than 0.999 8. The detection limits are 0.1-1.0 mg/kg. This method can be used exclusively and quickly to screen and confirm ten anti-acne compounds added in anti-acne cosmetics. It is mainly suitable for the simultaneous determination of ten anti-acne compounds in anti-acne cosmetics.

Key words: high performance liquid chromatography, liquid chromatography-tandem mass spectrometry, anti-acne cosmetics, anti-acne

中图分类号:

TQ658

张珊珊,贾昌平. 高效液相色谱法同时测定祛痘类化妆品中的10种抗痤疮类化学成分及质谱确证[J]. 日用化学工业（中英文）, 2022, 52(10): 1140-1146.

Zhang Shanshan,Jia Changping. Simultaneous determination of ten anti-acne compounds in anti-acne cosmetics by high performance liquid chromatography and verification by liquid chromatography-tandem mass spectrometry[J]. China Surfactant Detergent & Cosmetics, 2022, 52(10): 1140-1146.

图/表 7

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参考文献 10

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时间/min	φ（A）/%	φ（B）/%
0	30	70
4.0	10	90
5.0	10	90
7.0	5	95
7.1	30	70
10.0	30	70

序号	化合物名称	ESI+/-	保留时间/min	母离子	碰撞能量/eV	子离子
1	螺内酯	+	1.045	341.210 9	35	107.085 4,91.054 2
2	他扎罗汀	+	3.495	352.136 7	30	324.106 3,294.059 3
3	他卡西醇	+	3.652	417.330 6	15	399.326 8,381.314 6
4	依曲替酯	+	5.513	355.227 3	15	309.185 5,205.122 7
5	维胺酯	+	5.894	448.283 7	25	283.204 4,161.094 8
6	过氧苯甲酰	-	1.636	121.030 1	10	77.040 5
7	阿维A	-	3.913	325.181 1	20	266.165 2,119.087 0
8	异维甲酸	-	4.452	299.201 3	15	255.211 3,119.086 7
9	维甲酸	-	4.610	299.201 3	25	255.211 3,119.086 6
10	阿达帕林	-	5.589	411.196 0	40	352.177 9,367.204 1

编号	化合物名称	线性范围/（mg/L）	回归方程	相关系数r	LOD/（mg/kg）	LOQ/（mg/kg）
1	螺内酯	1.0~200	Y=22 261X-7 935	0.999 9	0.2	0.7
2	过氧苯甲酰	1.0~200	Y=43 399X-13 060	0.999 9	0.1	0.2
3	他卡西醇	0.1~20	Y=18 917X-485	0.999 9	1.0	3.5
4	他扎罗汀	0.5~100	Y=53 441X-4 884	0.999 9	0.4	1.4
5	阿维A	0.5~100	Y=76 346X-15 154	0.999 9	0.3	0.9
6	异维甲酸	0.5~100	Y=66 675X-4 838	0.999 9	0.3	0.8
7	维甲酸	0.5~100	Y=79 968X+3 258	0.999 8	0.2	0.7
8	维胺酯	0.5~100	Y=55 124X+5 394	0.999 9	0.3	0.9
9	依曲替酯	0.5~100	Y=68 977X-4 093	0.999 9	0.2	0.7
10	阿达帕林	0.2~40	Y=34 283X-588	0.999 9	0.5	1.5

化合物名称	加标水平/（mg/L）	平均回收率/%	RSD/%	化合物名称	加标水平/（mg/L）	平均回收率/%	RSD/%
螺内酯	2.0	93.3	0.7	异维甲酸	1.0	93.8	0.7
	40	100.6	1.9		20	97.7	1.2
	200	94.0	2.2		100	95.7	2.4
过氧苯甲酰	2.0	83.7	1.7	维甲酸	1.0	93.8	0.5
	40	93.4	2.0		20	96.8	1.2
	200	98.8	2.5		100	95.5	2.3
他卡西醇	0.2	90.9	2.6	维胺酯	1.0	80.8	0.4
	4.0	96.1	0.9		20	97.6	1.3
	20	96.5	2.5		100	96.3	2.3
他扎罗汀	1.0	95.3	0.8	依曲替酯	1.0	102.7	0.5
	20	92.1	2.1		20	97.7	1.2
	100	92.3	2.1		100	96.0	2.3
阿维A	1.0	93.1	0.6	阿达帕林	0.4	82.8	3.0
	20	97.3	1.3		8.0	98.0	1.2
	100	95.2	2.3		40	96.2	2.4

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