HPLC测定儿童化妆品中10种邻苯二甲酸酯类化合物的含量

Determination of 10 phthalate esters in cosmetics for children by HPLC

建立了测定儿童化妆品中10种邻苯二甲酸酯类(PAEs)化合物含量的高效液相色谱(HPLC)法。采用AcclaimTM 120-C18(4.6 mm×250 mm, 5 μm)反相柱,流动相为甲醇-乙腈-水,梯度洗脱,流速1.0 mL/min,二极管阵列检测器(DAD),检测波长280 nm。结果表明,在1～100 mg/L范围内,10种PAEs的质量浓度与峰面积呈现良好的线性关系,相关系数均≥0.999 6,10种PAEs的检出限和定量限分别在0.2～5.0 mg/L和0.5～10.0 mg/L范围内。方法验证过程中做了3类化妆品共计8种(化妆水、霜乳类和油状)样品的添加回收,平均回收率为89.2%～106.1%,RSD均小于5%。该方法简便准确,检测限较低,满足实际检测需要,可用于化妆品中PAEs的检测。1个样品有检出,通过3种方法确证为阳性。

A sensitive and rapid method was developed for the determination of 10 phthalate esters( PAEs) in children’s cosmetics by high performance liquid chromatography( HPLC). The analytes were tested with an AcclaimTM 120-C18 reversed-phase column( 4.6 mm×250 mm, 5 μm) under the gradient elution of methanol, acetonitrile and water, and subsequently detected by Diode Array Detector( DAD) at 280 nm. The flow rate was set at 1.0 mL/min. The results show that the ten compounds show good linearity within the concentration range of 1-100 mg/L. The corresponding linear correlation coefficients are all equal to or greater than 0.999 6. And the limits of detection and quantification( LOD and LOQ) located at the range of 0.2-5.0 mg/L and 0.5- 10.0 mg/L, respectively. Recovery experiments were then carried out with 8 cosmetic samples( lotion, cream and oily cosmetics). The average recoveries are between 89.2% and 106.1% with relative standard deviations <5%. Results show that it is a simple and accurate method with low LOD which can serve for cosmetics supervision in determination of the PAEs. One of the eight cosmetics was verified as a positive sample, and three methods were applied to confirm this result.