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建立了洗涤用品和化妆品护理用品中烷基酚聚氧乙烯醚(NPnEO和OPnEO,n=0~30)的高效液相色谱分析方法。采用乙腈水溶液超声提取不同基质类型的洗涤用品和化妆品护理用品,利用快速反相C18柱(Poroshell 120 EC-C18,75 mm×4.6 mm,2.7μm)串联HILIC硅胶色谱柱(Atlantis HILIC Slica,250 mm×4.6 mm,5μm)对NPnEO和OPnEO的各单体及样品杂质进行有效分离,以乙腈-10 mmol/L醋酸铵溶液为流动相进行梯度洗脱,荧光检测器进行检测,建立了荧光摩尔吸收系数定量校正NPnEO和OPnEO的计算模型。通过测定NPnEO和OPnEO混合标准溶液,计算得到两者的荧光摩尔吸收系数。对样品中NPnEO和OPnEO的平均分子量进行测定,并利用荧光摩尔吸收系数对总峰面积进行校正定量。方法的回收率为99.0%~105.7%,相对标准偏差不大于12.5%,定量下限为40.0 mg/kg。该方法快速、准确、适用范围广,可用于各类洗涤用品和化妆品护理用品中烷基酚聚氧乙烯醚(NPnEO和OPnEO)含量的检测。
A high performance liquid chromatographic method for the determination of alkylphenol ethoxylates (NPnEO and OPnEO, n = 0 to 30) in detergent and cosmetic care products was established. The samples were washed with acetonitrile aqueous solution and cleaned up with different matrix types of cleaning products and cosmetic care products. The samples were separated on a HILIC Silica gel column (Poroshell 120 EC-C18, 75 mm × 4.6 mm, 2.7 μm) using a reversed phase C18 column (Atlantis HILIC Slica, 250 mm × 4.6 mm, 5 μm). The monomer and sample impurities of NPnEO and OPnEO were separated effectively. The gradient elution was carried out with acetonitrile-10 mmol / L ammonium acetate solution as the mobile phase. The fluorescence detector was used to establish the fluorescence molar absorption Coefficient Quantitative Correction Models for NPnEO and OPnEO Calculation. By measuring the NPnEO and OPnEO mixed standard solution, calculate the fluorescence molar absorption coefficient of the two. The average molecular weights of NPnEO and OPnEO in the sample were determined, and the total peak area was corrected and quantified using the fluorescence molar absorption coefficient. The recoveries of the method were 99.0% -105.7%, the relative standard deviations were less than 12.5%, and the lower limit of quantitation was 40.0 mg / kg. The method is rapid, accurate and suitable for a wide range of applications. It can be used to detect the content of alkylphenol ethoxylates (NPnEO and OPnEO) in various detergent products and cosmetic products.