固相萃取/高效液相色谱法同时测定化妆品中13种防晒剂

利用反相高效液相色谱法建立了同时测定化妆品中13种防晒剂含量的检测方法。样品首先用5 mL二氯甲烷进行溶解,超声提取30min,经过硅胶固相萃取柱(500 mg,6 mL)净化,用5 mL正己烷-二氯甲烷(1∶1,V/V)洗脱淋洗,收集淋洗液上机。以Diamonsil C18柱(250 mm×4.6mm,5μm)为分离色谱柱,甲醇和0.5%(v/v)甲酸水溶液为流动相,梯度洗脱,以311 nm和254 nm为检测波长进行定性,外标法定量。各组分在0.5~1000 mg/L范围内成线性关系,相关系数0.99,平均回收率在84.96%~108.62%,相对标准偏差(n=6)为1.39%~7.65%。该方法样品分离效果好、成本低、回收率和重现性好,适用于化妆品中13种防晒剂的同时测定。

Determination of 13 Ultra-violet Absorbents in Cosmetics by SPE/high Performance Liquid Chromatography

A SPE/high liquid chromatography （HPLC） method was developed for the determination of 13 ultra-violet absorbents in cosmetics. The cosmetic samples were extracted by dichloromethane and ultrasonic extract 30 min, purification using a Si SPE（500 rag,6 nk） and 5mL n-hexane-dichloronethane（l：l.v/v）. The target compounds were separated of an Diamosil C18 column（250 mm×4.6 mm, 5 μm） in gradient elution made using methanol and 0.5 %（V/V） formic acid aqueous solution as mobile phase. The detective wavelength was 311 nm and 254 nm. The calibration curves showed good lineareties in the range of 0.5-1000 mg/L with correlation coefficients （r） larger than 0.99. The average recoveries were 84.96 %-108.62 % with relative standard deviations （RSD,n=6） of 1.39 %-7.65 %. The method is simple processing operations, low cost, have good recovery and reproducibility. The method can be used to determination 13 kinds of ultra-violet absorbents in cosmetics simultaneously.