高效液相色谱法测定防晒类化妆品中西诺沙酯等31种防晒剂的含量

Determination of cinoxate and other 30 kinds of sunscreen agents in sunscreen cosmetics by HPLC

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  sunscreen cosmetic  sunscreen agents  Cinoxate  Polysiloxane-15  content determination

摘要:

摘要 目的：建立防晒类化妆品中西诺沙酯等31种防晒剂的高效液相色谱检测方法。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（4.6×250mm,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 （2.1mm×100mm,3.5μm）色谱柱分离聚硅氧烷-15（21#）、Waters Symmetry C18（4.6×250mm,5μm）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#）、295nm（23～25#、27～31#）、311nm（其余成分），进样量5μL（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＞0.9999)，各成分的检测限范围在0.002~0.02%，两个基质在3个不同添加水平的加标回收率为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，其中聚硅氧烷-15检出10批。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。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。 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

Abstract:

Abstract Objective: To establish a method for determination cinoxate and other 30 kinds of sunscreen agents in sunscreen cosmetics by HPLC. Methods: 21 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 × 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 wasused to separate polysiloxane-15(21 #) , Waters Symmetry C18(4.6 × 250 mm, 5μm) 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, 1.0mL·min-1, The detection wavelengths were 358nm (7 # 、11 #) ,295nm（23～25#、27～31#), 311nm (other components) .The injection volumes of were 5μL（polysiloxane-15）and 10μL( 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 RSD of 0.02%~ 4.5%. 40 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 metho, the stability of drometrizole trisiloxan was improved,cinoxate, polysiloxane-15 and other7 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.