超高效液相色谱法检测化妆品中邻苯二甲酸酯

Determination of phthalates in cosmetic by ultra performance liquid chromatography

建立了测定化妆品中4种邻苯二甲酸酯-邻苯二甲酸二甲酯（DMP），邻苯二甲酸二乙酯（DEP），邻苯二甲酸二丁酯（DBP），和邻苯二甲酸二（2-乙基己基）酯（DEHP）-的分析方法。用超高效液相色谱（UPLC）带PDA检测器，色谱柱：Acquity UPLC^TM BEHC C18（50mm×2．1mm i．d．，1．7μm）。样品经乙腈提取后，用UPLC—PDA进行分析检测，结合保留时间和光谱进行定性分析，定量检测波长224nm。该法的回收率为94．3％-98．7％，精密度RSD为0．9％。2．6％，以10倍噪声计，DMP、DEP、DBP和DEHP的检出限分别为0．14、0．21、0．21、0．31ng。用该分析方法对115件化妆品样品进行了分析检测，29件化妆品检出DEP，14件DBP，25件DEHP。总检出阳性样品54件，总阳性检出率47．0％。其检出质量分数：2．5—4348．2μg／g。该方法分离效果好，灵敏度高，能够满足检测化妆品中4种邻苯二甲酸酯的需要。

To setup the method for the determination of 4 phthalates （dimethyl, diethyl, dibutyl, and di（2-ethylhexyl）, phthalate （respectively designated DMP, DEP, DBP, and DEHP）） in cosmetic, 4 phthalates in cosmetic were determined by ultra performance liquid chromatography （UPLC） with PDA detector. Chromatographic column： Acquity UPLCTM BEHC C18 （50 mm × 2.1 mm i.d., 1.7 μm）; After extracted by solvent CHBCN, Phthalates were detected by UPLC-PDA. The qualification analysis was done by using retention time and spectrum, and quantification was based on detection wavelength at 224 rim. The recoveries for phthalates in cosmetic were 94.3 % - 98.7 %. Relative standard deviations were 0.9% - 2.6%. The limits of detection （S/N = 10） for DMP, DEP, DBP, DEHP were 0.14, 0.21, 0.21 and 0.31 ng, respectively. 115 pieces of cosmetic samples were detected by this method. It was found that 29 samples contained DEP; 14 samples contained DBP; and 25 samples contained DEHP. The total 54 samples showed positive results. Total detectable rate of phthalates was 47.0%. The concentrations of phthalates were from 2.5 μg/g to 4348.2 μg/g. Results showed that the method was simple and fast, had a good separation effect and high sensitivity. So it can meet the demand for the determination of 4 phthalates in cosmetic.