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    高效液相色谱法测定化妆品和洗涤剂中5种荧光增白剂的含量

    Determination of 5 Fluorescent Whitening Agents in Cosmetics and Detergent by High Performance Liquid Chromatography

    • 摘要: 采用高效液相色谱法测定化妆品和洗涤剂中荧光增白剂C.I.85,C.I.210,C.I.220,C.I.351和C.I.353。1.000 g化妆品样品或0.500 g洗涤剂样品加入10.0 mL乙腈(1+2)溶液,涡旋振荡1 min后超声提取10 min,以10 000 r·min-1转速离心5 min,上清液经0.22 μm滤膜过滤后,在MG C18色谱柱(250 mm×4.6 mm,5 μm)上分离,以乙腈和含2 mmol·L-1乙酸二正己基铵的10 mmol·L-1乙酸铵溶液为流动相进行梯度洗脱,采用二极管阵列检测器,在波长350 nm处进行检测。5种荧光增白剂的质量浓度均在5.0~100 mg·L-1内与对应的色谱峰面积呈线性关系,检出限(3S/N)在4~20 mg·kg-1之间,测定下限(10S/N)在15~70 mg·kg-1之间。对空白样品在5.0,50,100 mg·L-1等3个浓度水平上进行加标回收试验,回收率在80.3%~111%之间。对样品中的5种荧光增白剂进行6次平行测定,测定值的相对标准偏差在2.4%~8.9%之间。

       

      Abstract: A method of high performance liquid chromatography was developed to determine 5 fluorescent whitening agents, including C.I. 85, C.I. 210, C.I. 220, C.I. 351 and C.I. 353, in cosmetics and detergent. The sample (1.000 g of cosmetics or 0.500 g of detergent) was mixed well with 10.0 mL of acetonitrile (1+2) solution by vortex oscillation for 1 min, and then ultrasonically extracted for 10 min. After the mixture was centrifugated at 10 000 r·min-1 for 5 min, the supernatant was filtered through a 0.22 μm filter membrane, and seperated on a MG C18 column (250 mm×4.6 mm, 5 μm), with a mixture of acetonitrile and 10 mmol·L-1 ammonium acetate solution (containing 2 mmol·L-1 di-n-hexyl-ammonium acetate) for gradient elution. A diode array detector was used for detection at the wavelength of 350 nm. Linear relationships were found between peak areas and mass concentrations of the 5 fluorescent whitening agents in the same range of 5.0-100 mg·L-1, with detection limits (3S/N) in the range of 4-20 mg·kg-1, and lower limits of determination (10S/N) in the range of 15-70 mg·kg-1. Tests for recovery was made to blank samples at mass contentrations of 5.0, 50, 100 mg·L-1, giving values of recovery between 80.3% and 111%. The 5 fluorescent whitening agents in the samples were determined in parallel for 6 times, and the relative standard deviations of the measured values were between 2.4% and 8.9%.

       

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