柱后衍生-高效液相色谱法测定化妆品中游离甲醛

摘要

建立了化妆品中游离甲醛的测定方法。样品经0.2%（质量分数，下同）磷酸溶液提取，高效液相色谱分离，柱后衍生测定，外标法进行定量，阳性样品用高效液相色谱-三重四级杆串联质谱进行确证。采用INERTSIL ODS-SP色谱柱（25 cm×0.46 cm×5μm），流动相为0.2%磷酸溶液，流速1.0 mL/min，检测波长为420 nm，柱温20℃，柱后衍生溶液流速0.5 mL/min，衍生温度100℃。甲醛在1～50μg/mL范围内线性关系良好，r>0.999。回收率为96.4%～106.6%，检出限为0.003%。该方法快速简便，可用于化妆品中游离甲醛的定量分析。%A determination method for free formaldehyde in cosmetics by HPLC with post - column derivation was established. Samples were prepared by 0.2%(mass fraction) phosphoric acid solution. After separated by high performance liquid chromatogram and derived with acetyl acetone, the derivate was determined by DAD detector with external standard method. Positive samples were confirmed by LC-MS/MS. The separation was carried out on an INERTSIL ODS - SP column(25 cm × 0.46 cm× 5μm) with 0.2% phosphoric acid as the mobile phase. The rate was 1.0 mL/min, the detection wavelength was 420 nm and the column temperature was 20℃. The rate of derivation solution was 0.5 mL/min and the derivation temperature was100℃. Free formaldehyde showed a good linear relationship at a range of 1-50μg/mL(r>0.999). The recovery was 96.4% to 106.6%, the detection limit was 0.003%. This method is rapid, simple, and can be used for quantified determination of free formaldehyde in cosmetics.