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    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

      摘要
    • 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，5 µm)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、1.0 mL·min−1，检测波长为358 nm(7#、11#)、295 nm(23#~25#、27#~31#)、311 nm(其余成分)，进样量5 µL(聚硅氧烷-15)、10 µL(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>0.9999) 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.

       

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