液质联用法同时测定化妆品中辛酰羟肟酸、对羟基苯乙酮、p-茴香酸的含量

doi:10.3969/j.issn.2097-2806.2023.05.015

摘要/Abstract

摘要：

采用高效液相色谱-三重四极杆质谱联用仪同时检测化妆品中辛酰羟肟酸、对羟基苯乙酮、p-茴香酸的含量，以0.1%乙酸-乙腈（含0.1%甲酸）为流动相，采用梯度洗脱的方式，根据保留时间和特征离子对的相对丰度比进行定性，以特征离子的峰面积进行定量，用标准曲线法计算三种物质的含量。结果显示，水、乳、霜三种基质中辛酰羟肟酸、对羟基苯乙酮、p-茴香酸分别在10~2 000，2~2 000和5~2 000 ng/mL时，与峰面积呈现良好的线性关系，相关系数（r）>0.999。该方法测定化妆品中辛酰羟肟酸、对羟基苯乙酮、p-茴香酸于48 h内稳定，回收率在87.37%~111.56%之间，精密度的平均相对标准偏差（RSD）分别为1.4%，1.8%和1.6%。该检测方法高效、方便且定性定量准确，适用于不同基质化妆品中辛酰羟肟酸、对羟基苯乙酮、p-茴香酸的定量定性分析。

关键词: 液质联用法, 化妆品, 辛酰羟肟酸, 对羟基苯乙酮, p-茴香酸

Abstract:

The content of caprylhydroxamic acid, 4-hydroxyacetophenone and p-anisic acid in cosmetics was simultaneously determined by HPLC-MS. The mobile phase was 0.1% acetic acid in acetonitrile （containing 0.1% formic acid） by using the gradient elution method. The qualitative analysis of these components was based on the retention time and the relative abundance ratio of the characteristic ion pairs. The peak area of the characteristic ions was used for quantitative analysis. The standard curve method was used to calculate the content of the three substances. The results showed that, in liquid matrix, lotion matrix and cream matrix, caprylhydroxamic acid, 4-hydroxyacetophenone and p-anisic acid showed good linear relationships in the range of 10-2 000, 2-2 000 and 5-2 000 ng/mL, respectively, while the correlation coefficients （r） were>0.999. This method was applied to determine the caprylhydroxamic acid, 4-hydroxyacetophenone and p-anisic acid in cosmetics, the results of which were stable within 48 hours. The recovery rates were between 87.37% and 111.56%. The average relative standard deviation （RSD） of the precision research was 1.4%, 1.8% and 1.6%, respectively. This method is efficient, convenient, and accurate in qualitative and quantitative analysis. It is suitable for quantitative and qualitative analysis of caprylhydroxamic acid, 4-hydroxyacetophenone and p-anisic acid in cosmetics of different matrices.

Key words: HPLC-MS, cosmetics, caprylhydroxamic acid, 4-hydroxyacetophenone, p-anisic acid

中图分类号:

TQ658

李泽夏琼, 邱红燕, 马莹, 刘丹, 赵丽. 液质联用法同时测定化妆品中辛酰羟肟酸、对羟基苯乙酮、p-茴香酸的含量[J]. 日用化学工业（中英文）, 2023, 53(5): 596-601.

Li Zexiaqiong, Qiu Hongyan, Ma Ying, Liu Dan, Zhao Li. Simultaneous determination of caprylhydroxamic acid, 4-hydroxyacetophenone and p-anisic acid in cosmetics by HPLC-MS[J]. China Surfactant Detergent & Cosmetics, 2023, 53(5): 596-601.

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参考文献 14

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序号	物质名称	电离方式	母离子/（m/z）	Frag./V	子离子/（m/z）	CE/V
1	对羟基苯乙酮	ESI⁺	136.95	23	42.7^*	13
1	对羟基苯乙酮	ESI⁺	136.95	23	94.7	10
2	辛酰羟肟酸	ESI⁺	160.05	29	56.75^*	15
2	辛酰羟肟酸	ESI⁺	160.05	29	103.8	13
3	p-茴香酸	ESI⁺	152.987	22	108.82^*	13
3	p-茴香酸	ESI⁺	152.987	22	93.8	18

物质名称	回归方程	相关系数r	检出限/（ng/mL）	定量限/（ng/mL）	线性范围/（ng/mL）
辛酰羟肟酸	y=1 207x-858	0.999 6	3.16	10.52	10.52~2 094.00
对羟基苯乙酮	y=1 602x+39 442	0.999 5	0.61	2.02	2.02~2 031.97
p-茴香酸	y=1 050x-1 994	0.999 2	1.52	5.06	5.06~2 017.98

成分	加标质量浓度/（ng/mL）	实测平均质量浓度/（ng/mL）			回收率/%
成分	加标质量浓度/（ng/mL）	水基质	乳基质	霜基质	水基质	乳基质	霜基质
辛酰羟肟酸	52.35	47.89	47.87	54.70	91.49	91.45	104.48
		46.85	48.12	53.11	89.50	91.92	101.45
		46.77	48.79	51.46	89.33	93.20	98.31
	523.50	483.52	488.04	472.87	92.36	93.23	90.33
		473.36	461.68	480.75	90.42	88.19	91.83
		466.26	477.29	472.75	89.07	91.17	90.30
	1 047.00	987.57	983.89	962.36	94.32	93.97	91.92
		956.72	1 037.90	971.01	91.38	99.13	92.74
		944.41	960.80	965.01	90.20	91.77	92.17
对羟基苯乙酮	50.80	47.62	48.22	48.52	93.74	94.92	100.62
		48.15	45.03	48.27	94.78	88.64	107.20
		48.27	47.77	48.41	95.02	94.04	101.34
	507.99	501.72	476.47	506.82	98.77	93.80	99.77
		491.40	503.12	496.97	96.73	99.04	97.83
		498.05	505.18	501.67	98.04	99.45	98.76
	1 015.98	892.67	888.64	887.71	87.86	87.47	87.37
		953.15	939.04	932.92	93.82	92.43	91.82
		926.68	945.85	951.00	91.21	93.10	93.60
p-茴香酸	50.45	52.63	55.94	55.28	104.32	110.87	109.58
		55.17	54.33	54.39	109.35	107.68	107.80
		55.61	55.10	56.28	110.22	109.21	111.56
	504.50	451.81	457.93	485.66	89.56	90.77	96.27
		461.64	474.77	472.86	91.50	94.11	93.73
		455.14	448.89	462.62	90.22	88.98	91.70
	1 008.99	1 053.48	937.17	1 008.43	104.41	92.88	99.94
		1 022.13	926.05	1 015.53	101.30	91.78	100.65
		1 007.18	974.35	972.56	99.82	96.57	96.39

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