首页|超高效液相色谱法测定化妆品中聚硅氧烷-15等7种脂溶性防晒剂的含量

超高效液相色谱法测定化妆品中聚硅氧烷-15等7种脂溶性防晒剂的含量

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建立了一种超高效液相色谱法测定聚硅氧烷-15等7种脂溶性防晒剂含量的方法,样品使用乙醇-四氢呋喃(体积比3∶1)混合溶剂超声提取,经Waters Symmetry C18(150×4.6 mm,3.5 μm)色谱柱分离,以异丙醇-四氢呋喃(体积比90∶10)-水为流动相进行梯度洗脱,流速0.7 mL/min,柱温为25 ℃,检测波长311 nm.结果表明,7种脂溶性防晒剂在相应的质量浓度范围内线性关系良好(r≥0.9999),不同基质类型的样品在低、中、高3个浓度水平的平均加标回收率为94.4%~103.0%,相对标准偏差为0.4%~4.4%,检出限和定量限范围分别为0.002%~0.009%和0.005%~0.03%,各成分在48 h内稳定.采用该方法测定市售30批化妆品中的防晒剂,测定结果与《化妆品安全技术规范》(2015版)方法相比,检出的亚甲基双-苯并三唑基四甲基丁基酚、双-乙基己氧苯酚甲氧苯基三嗪等脂溶性防晒剂提取效果优于《规范》方法.该方法准确、快速、灵敏度高、稳定性好,可用于化妆品中脂溶性防晒剂的测定.
Determination of Polysilicone-15 and Other Six Kinds of Fat-soluble Sunscreen in Cosmetics by Ultra-High Performance Liquid Chromatography
An ultra-high performance liquid chromatography method was developed for the determination of 7 kinds of fat-soluble sunscreen agents containing polysilicone-15.The samples were ultrasonic extracted by ethanol-tetrahydrofuan(3∶1,V/V)mixed solution for determination.The determination was performed by gradient elution with isopropanol-tetrahydrofuran(90∶10,V/V)-water as the mobile phase on a Waters Symmetry C18(4.6×150 mm,3.5 μm)analytical column.The flow rate was 0.7 mL/min,the column temperature was 25 ℃,and the wavelength was 311 nm.The developed method showed good linear relationships,with correlation coefficients(r)of no less than 0.9999 in corresponding concentration ranges.The average spiked recoveriers of different substrates at three levels ranged from 94.4%to 103.0%,with the relative standard deviations(RSDs)ranging from 0.4%to 4.4%.The limits of detection were between 0.002%and 0.009%,and the limits of quantification ranged from 0.005%to 0.03%.Moeroever,all the analytes were stable within 48h.By applying the developed method to 30 cosmetic samples obtained from the Chinese market,the extraction efficiency of fat-soluble sunscreen agemts such as methylene bis-benzotriazolyl tetramethylbutylphenol and bis-ethylhexyloxyphenol methoxyphenyl triazine were greatly improved comparing with current method in Technical Specification for Safety of Cosmetics(2015 edition).The method is accurate,rapid,sensitive and stable,which is suitable for the determination of fat-soluble sunscreens in cosmetics.

Ultra-high performance liquid chromatographyCosmeticsPolysilicone-15Tris-biphenyl triazineSunscreen

郭珊珊、简育莹、卓婧、陈硕、卢端萍

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福建省食品药品质量检验研究院,福建福州 350012

超高效液相色谱法 化妆品 聚硅氧烷-15 三联苯基三嗪 防晒剂

2024

分析科学学报
武汉大学,北京大学,南京大学

分析科学学报

CSTPCD北大核心
影响因子:0.717
ISSN:1006-6144
年,卷(期):2024.40(1)
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