超声提取-高效液相色谱法测定化妆品中5种苯并三唑类紫外线吸收剂

doi:10.3969/j.issn.1001-1803.2023.01.015

摘要/Abstract

摘要：

建立了一种利用高效液相色谱同时测定化妆品中甲酚曲唑（UV-P）、奥克三唑（UV-329）、布美三唑（UV-326）、甲酚曲唑三硅氧烷（DTTSO）、亚甲基双-苯并三唑基四甲基丁基酚（UV-360）的方法。其中，水状化妆品经甲醇/四氢呋喃溶解、超声提取、微孔滤膜过滤后进样；乳液状、霜状化妆品经甲醇/四氢呋喃溶解、涡旋振荡、超声提取、微孔滤膜过滤后进样。使用ZORBAX SC-C18色谱柱（250 mm×4.6 mm，5 μm），柱温23 ℃，以0.1%的甲酸水溶液为A相、甲醇为B相、四氢呋喃为C相进行洗脱，流速1.0 mL/min，检测波长340 nm，进样量5 μL。结果表明，5种紫外线吸收剂在11~176 mg/L的质量浓度范围内线性关系良好（R²≧0.999 4），检测限分别为6.72，11.94，13.80，18.47和23.49 μg/L，相对标准偏差小于1.7%（n=6），加标平均回收率达到93.7%~104.5%。该方法能满足化妆品中5种苯并三唑类紫外线吸收剂的测定。

关键词: 超声提取, 高效液相色谱, 化妆品, 苯并三唑, 防晒剂, 紫外线吸收剂

Abstract:

A method for the determination of 2-（2-benzotriazolyl）-4-methylphenol（UV-P）, 2-benzotriazol-2-yl-4-（1, 1, 3, 3-tetramethylbutyl）phenol（UV-329）, 2-tert-butyl-6-（5-chloro-2H-benzotriazol-2-yl）-4-methylphenol（UV-326）, 2-（benzotriazol-2-yl）-4-methyl-6-[2-methyl-3-[methyl-bis（trimethylsilyloxy）silyl]propyl]phenol（DTTSO） and 2, 2-methylenebis[6-（2H-benzotriazol-2-yl）-4-（1, 1, 3, 3-tetramethylbutyl）phenol]（UV-360） in cosmetics by high performance liquid chromatography was established. Watery cosmetics were dissolved in methanol/tetrahydrofuran, ultrasonically extracted, and filtered by microporous membrane for injection. Emulsion and cream cosmetics were prepared by methanol/tetrahydrofuran dissolution, vortex oscillation, ultrasonic extraction, and microporous membrane filtration injection. The target chemicals were separated on ZORBAX SC-C18 column（250 mm×4.6 mm, 5 μm）using 0.1% formic acid, methanol and tetrahydrofuran as mobile phases and detected at 340 nm and 23 ℃. The flow rate of the mobile phase was 1.0 mL/min and the injection volume was 5 μL. The results show that the five benzotriazole ultraviolet absorbents have a good linear relationship in the mass concentration range of about 11-176 mg/L（R²≧0.999 4）, the detection limits are 6.72, 11.94, 13.80, 18.47 and 23.49 μg/L, respectively, the relative standard deviation is less than 1.7%（n=6）, and the average recovery rate is 93.7%-104.5%. The method is suitable for the determination of five benzotriazole ultraviolet absorbents in cosmetics.

Key words: ultrasonic extraction, high performance liquid chromatography, cosmetic, benzotriazole, sunscreen, ultraviolet absorbent

中图分类号:

TQ658

王磊, 吴越, 田冬. 超声提取-高效液相色谱法测定化妆品中5种苯并三唑类紫外线吸收剂[J]. 日用化学工业（中英文）, 2023, 53(1): 109-114.

Wang Lei, Wu Yue, Tian Dong. Determination of five benzotriazole UV absorbers in cosmetics by ultrasonic extraction and high performance liquid chromatography[J]. China Surfactant Detergent & Cosmetics, 2023, 53(1): 109-114.

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参考文献 11

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化合物	保留时间/min	分离度	理论塔板数
UV-P	3.03	—	8 614
UV-329	3.70	4.71	8 494
UV-326	4.32	3.80	9 709
UV-360	5.06	3.83	8 552
DTTSO	6.17	4.32	7 052

化合物	线性方程	R²	质量浓度范围/（mg/L）	检出限/（μg/L）
UV-P	y=9.800 1x+11.154 9	0.999 4	11.00~176.0	6.72
UV-329	y=7.091 8x+7.047 0	0.999 7	11.30~180.8	11.94
UV-326	y=7.260 9x+7.728 0	0.999 6	11.50~184.0	13.80
UV-360	y=7.132 1x+13.948 2	0.999 5	11.00~176.0	18.47
DTTSO	y=4.859 5x+1.288 4	0.999 4	11.10~177.6	23.49

化合物	加标量	回收率/%						平均回收率/%	RSD/%
化合物	加标量	1	2	3	4	5	6	平均回收率/%	RSD/%
UV-P	低	99.82	99.37	98.64	100.68	99.71	100.53	99.8	0.8
	中	97.36	98.06	98.37	96.05	99.78	97.07	97.8	1.3
	高	102.93	100.26	102.97	102.27	101.06	102.48	102.0	1.1
UV-329	低	98.23	95.22	95.10	96.04	98.70	95.46	96.5	1.7
	中	99.93	98.61	98.27	98.11	98.73	100.06	99.0	0.9
	高	96.63	96.89	95.07	98.16	95.22	95.45	96.2	1.3
UV-326	低	97.88	99.63	98.54	100.29	98.14	99.52	99.0	1.0
	中	97.02	97.26	99.48	101.25	98.43	99.17	98.8	1.6
	高	100.06	101.28	101.40	101.71	101.66	101.14	101.2	0.6
DTTSO	低	92.61	94.76	92.34	93.28	94.29	94.97	93.7	1.2
	中	97.54	99.82	97.88	99.36	98.38	97.06	98.3	1.1
	高	95.83	95.44	94.03	95.39	94.62	96.37	95.3	0.9
UV-360	低	97.66	95.47	96.56	96.63	96.07	97.92	96.7	1.0
	中	99.52	101.86	101.39	101.46	98.13	100.54	100.5	1.4
	高	104.77	103.39	104.56	103.46	104.90	105.67	104.5	0.9

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