HPLC-MS/MS测定化妆品中14种荧光增白剂

    Determination of Fourteen Fluorescent Whitening Agents in Cosmetics by HPLC-MS/MS

    • 摘要: 目的 建立HPLC-MS/MS定量测定化妆品中14种荧光增白剂的分析方法。方法 样品经N,N-二甲基甲酰胺超声提取,选用Waters ACQUITY UPLC ®BEH C18(2.1 mm×50 mm,1.7 μm)色谱柱,以甲醇-0.1%氨水水溶液梯度洗脱,流速0.3 mL·min-1,柱温40 ℃;质谱法采用三重四级杆质谱,电喷雾离子源,在正/负离子、多反应监测模式下进行扫描。结果 14种荧光增白剂在定量范围内线性关系良好,相关系数均>0.99,定量限为0.01~20 μg·g-1,检出限为0.004~ 8 μg·g-1;在3个添加水平下的平均回收率为85.4%~108.9%,相对标准偏差为0.3%~7.2%。结论 该方法灵敏度高,专属性强,操作简单方便,适用于化妆品中14种荧光增白剂的含量测定。

       

      Abstract: OBJECTIVE To establish a method for the determination of fourteen fluorescent whitening agents in cosmetics by HPLC-MS/MS. METHODS Samples were extracted on a Waters ACQUITY UPLC ®BEH C18(2.1 mm×50 mm, 1.7 μm) column after ultrasonic extracted by DMF with the mobile phase consisted of methanol-0.1% ammonia water solution by gradient elution. The flow rate was 0.3 mL·min-1. The column temperature was 40 ℃. MS was performed using triple quadrupole mass spectrometry. Electrospray ionization source was operated in the positive/negative mode using multiple reaction monitoring scanning mode. RESULTS The results showed that there were good linear relationships for the fluorescent whitening agents in a certain concentration range with correlation coefficients(r) greater than 0.99. The limits of quantification were 0.01-20 μg·g-1 and the limits of detection were 0.004-8 μg·g-1. The average recoveries at three spiked levels were in the range of 85.4%-108.9%, and the relative standard deviation were in the range of 0.3%-7.2%. CONCLUSION The method has high sensitivity, strong specificity, simple and convenient operation, and is suitable for the detection of fourteen fluorescent whitening agents in cosmetics.

       

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