HPLC测定防晒类化妆品中西诺沙酯等31种防晒剂的含量
Determination of 31 Kinds of Sunscreen Agents Including Cinoxate in Sunscreen Cosmetics by HPLC
卢端萍 1郭珊珊 1程佳华 1张丽蓉 1韩康印 1陈硕1
作者信息
- 1. 福建省食品药品质量检验研究院,福州 350012
- 折叠
摘要
目的 建立防晒类化妆品中西诺沙酯等31种防晒剂的HPLC检测方法.方法 样品以甲醇-四氢呋喃(1∶1)混合溶液超声提取21种脂溶性防晒剂(1#～21#),以甲醇-四氢呋喃-水(2∶3∶5)混合溶液超声提取10种水溶性防晒剂(22#～31#),采用Agilent ZORBAX SB C18(4.6 mm×250 mm,5μm)色谱柱分离西诺沙酯等20种脂溶性防晒剂(1#～20#)、Agilent ZORBAX SB C18(2.1 mm×100 mm,3.5 μm)色谱柱分离聚硅氧烷-15(21#)、Waters Symmetry C18(4.6 mm×250 mm,5 μm)色谱柱分离10种水溶性防晒剂,分别以甲醇-异丙醇-水、异丙醇-四氢呋喃-水、甲醇-乙腈-0.02 mol·L-1乙酸铵溶液(加磷酸调pH值至5.0)为流动相进行梯度洗脱,流速分别为1.2、0.5、1.0mL·min-1,检测波长为358nm(7#、11#)、295 nm(23#～25#、27#～31#)、311 nm(其余成分),进样量5 μL(聚硅氧烷-15)、10μL(其余成分),柱温30℃.结果 31种防晒剂在考察的质量浓度范围内呈良好的线性关系(r＞0.999 9),各成分的检测限范围为0.002％～0.02％,2个基质在3个不同添加水平的加样回收率为92.4％～110.3％,RSD范围为0.02％～4.5％.应用该方法对40批国产及进口防晒类化妆品进行检测,结果检出17种准用防晒剂,其中有10批检出聚硅氧烷-15.与《化妆品安全技术规范》(2015版)现行方法相比,该方法改善了部分脂溶性的防晒剂的提取效率,提高了甲酚曲唑三硅氧烷的稳定性,同时增加了西诺沙酯、聚硅氧烷-15等9种防晒剂的检测.结论 本方法准确、灵敏、可靠,可用于防晒类化妆品中防晒剂的检测分析.
Abstract
OBJECTIVE To establish a method for determination cinoxate and other 30 kinds of sunscreen agents in sunscreen cosmetics by HPLC.METHODS Twenty-one fat-soluble sunscreen agents(1#-21#)were ultrasonically extracted by the mixed solution of methanol-tetrahydrofuran(1∶1),10 kinds of water-soluble sunscreen agents(22#-31#)were ultrasonically extracted by the mixed solution of methanol-tetrahydrofuran-water(2∶3∶5)from the samples.Agilent Zorbax SB C18(4.6 mm× 250 mm,5 μm)column was used to separate cinoxate and other fat-soluble sunscreen agents(1#-20#),Agilent Zorbax SB C18(2.1 mm× 100 mm,3.5 μm)column was used to separate polysiloxane-15(21#),Waters Symmetry C18(4.6 mm× 250 mm,5 μm)column was used to separate 10 water-soluble sunscreen agents.Methanol-isopropanol-water,isopropanol-tetrahydrofuran-water,and methanol-acetonitrile-0.02 mol·L-1 ammonium acetate solution(add phosphoric acid to adjust pH to 5.0)were used as mobile phase in gradient elution respectively.The flow rates were 1.2,0.5,1.0 mL·min-1.The detection wavelengths were 358nm(7 #,11#),295 nm(23#-25#,27#-31#),311 nm(other components).The injection volumes were 5 μL(polysiloxane-15)and 10 μL(other component),the column temperature was set at 30 ℃.RESULTS The linear relationships(r＞0.999 9)of 31 sunscreen agents were good in corresponding concentration range.The limit of detection were in the range of 0.002％-0.02％.The recoveries of two substrates at three different supplemental levels ranged from 92.4％to 110.3％,with the RSDs of 0.02％-4.5％.Forty batches of domestic and imported sunscreen cosmetics were determined by this method,17 kinds of approved sunscreen agents were detected,of which polysiloxane-15 were detected in 10 batches of samples.By comparing with the current method in Safety and Technical Standards for Cosmetics(2015 edition),it was found that the extraction efficiency of fat-soluble sunscreen agents was superior to the current method,the stability of drometrizole trisiloxan was improved,cinoxate,polysiloxane-15 and other 7 kinds of sunscreens were added.CONCLUSION This method is accurate,sensitive and reliable,which can be used for the detection and analysis of sunscreen in sunscreen cosmetics.
关键词
高效液相色谱法/化妆品/防晒剂/西诺沙酯/聚硅氧烷-15/含量测定Key words
HPLC/cosmetic/sunscreen agents/cinoxate/polysiloxane-15/content determination引用本文复制引用
基金项目
福建药品监督管理局科技计划项目(2023019)
出版年
2024
NETL
NSTL
万方数据