Determination of 31 Kinds of Sunscreen Agents Including Cinoxate in Sunscreen Cosmetics by HPLC
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.