高效液相色谱法同时测定化妆品中5种抗氧化成分

doi:10.3969/j.issn.1001-1803.2022.08.010

摘要/Abstract

摘要：

建立了高效液相色谱法同时测定化妆品中儿茶素、表儿茶素、没食子酸、芦丁、槲皮素含量的分析方法。待测物经CAPCELL PAK MG C₁₈色谱柱（4.6 mm×250 mm）分离,梯度洗脱;流动相为0.1%磷酸水溶液-甲醇,儿茶素、表儿茶素、没食子酸测定波长为280 nm,芦丁、槲皮素测定波长为360 nm,柱温为30 ℃,PDA检测器,流速1.0 mL/min。结果显示,儿茶素、表儿茶素、没食子酸、芦丁、槲皮素在0.594 5~15.403 6 μg/mL范围内线性良好,r>0.999。上述5种化合物的检出限范围为0.025 1~0.128 4 ng/mL,24 h内稳定性良好。水基质中的平均回收率为99.7%,乳霜基质中的平均回收率为99.4%。该方法操作简便,准确性良好,适用于同时测定化妆品中儿茶素、表儿茶素、没食子酸、芦丁、槲皮素5种成分含量。

关键词: 高效液相色谱法, 化妆品, 抗氧化, 双波长, 含量测定

Abstract:

This experiment adopts high performance liquid chromatography method to simultaneously detect the content of catechins, epicatechins, gallic acid, rutin and quercetin in cosmetics, and provides certain reference for the detection of antioxidant ingredients in plant extracts in cosmetics. Test samples were separated by CAPCELL PAK MG C₁₈ column （4.6 mm×250 mm） and underwent gradient elution. The mobile phase was 0.1% aqueous phosphate solution-methanol, the wavelength of catechins, epicatechins, and gallic acid was 280 nm and that of rutin and quercetin was 360 nm. The column temperature was 30 ℃ with the PDA detector, and the flow rate was 1.0 mL/min. The five compositions are linearly good in the range of 0.594 5-15.403 6 μg/mL, and the r>0.999. The detection limit of this method is 0.025 1-0.128 4 ng/mL. The average recovery rate in the water matrix is 92%-113%, and that in the cream matrix is 90%-110%. This method is easy to operate, and has good stability. Therefore, it is accurate and suitable for simultaneously measuring the content of catechins, epicatechins, gallic acid, rutin and quercetin in cosmetics.

Key words: high performance liquid chromatography, cosmetics, anti-oxidation, dual wavelengths, content determination

中图分类号:

TQ658

刘丹,何燕伶,邱红燕,马莹. 高效液相色谱法同时测定化妆品中5种抗氧化成分[J]. 日用化学工业, 2022, 52(8): 858-862.

Liu Dan,He Yanling,Qiu Hongyan,Ma Ying. Simultaneous determination of 5 antioxidant components in cosmetics by high performance liquid chromatography[J]. China Surfactant Detergent & Cosmetics, 2022, 52(8): 858-862.

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成分	线性方程	线性范围/（μg/mL）	相关系数r	检出限/（ng/mL）	定量限/（ng/mL）
儿茶素	Y=8 384x-1 849	0.620 5~14.892 7	0.999 9	0.124 1	0.413 7
表儿茶素	Y=9 369x-2 634	0.641 8~15.403 6	0.999 8	0.128 4	0.427 9
没食子酸	Y=34 913x-7 825	0.595 3~14.287 7	0.999 8	0.059 5	0.198 4
芦丁	Y=21 662x-2 782	0.594 5~14.267 5	0.999 8	0.059 4	0.198 2
槲皮素	Y=40 408x-7 995	0.628 1~15.074 8	0.999 8	0.025 1	0.083 7

成分	ρ/ （μg/mL）	水基质峰面积RSD/%	乳霜基质峰面积RSD/%
没食子酸	24.82 124.1	0.6 0.3	0.3 1.1
儿茶素	25.67 128.4	2.6 0.2	3.6 0.6
表儿茶素	25.67 128.4	3.4 0.5	2.9 0.3
芦丁	23.78 118.9	3.3 0.5	2.4 0.3
槲皮素	25.12 125.6	3.0 3.3	1.1 0.3

成分	加标质量浓度/（μg/mL）	称样量/g	实测平均质量浓度/（μg/mL）	平均回收率/%	RSD/%
没食子酸	7.144 119.100	0.5	7.468 110.100	105 92	1.8 1.7
儿茶素	7.446 124.100	0.5	8.103 117.700	109 95	2.0 1.8
表儿茶素	7.702 128.400	0.5	8.667 117.800	113 92	2.3 1.8
芦丁	7.134 118.900	0.5	7.073 113.800	99 96	4.2 1.6
槲皮素	7.537 125.600	0.5	7.512 122.300	100 97	4.6 1.8

成分	加标质量浓度/（μg/mL）	称样量/g	实测平均质量浓度（μg/mL）	平均回收率/%	RSD/%
没食子酸	7.144 119.100	0.5	7.453 109.100	104 92	1.9 1.6
儿茶素	7.446 124.100	0.5	8.007 116.500	108 94	1.3 1.5
表儿茶素	7.702 128.400	0.5	8.494 116.100	110 90	4.2 1.8
芦丁	7.134 118.900	0.5	6.789 112.500	95 95	2.1 1.6
槲皮素	7.537 125.600	0.5	8.129 123.700	108 98	4.7 1.9