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

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。1.000g化妆品样品或0.500g洗涤剂样品加入10.0mL乙腈(1+2)溶液,涡旋振荡1min后超声提取10min,以10 000r·min-1转速离心5min,上清液经0.22μm滤膜过滤后,在MG C18色谱柱(250mm×4.6mm,5μm)上分离,以乙腈和含2mmol·L^(-1)乙酸二正己基铵的10mmol·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350nm处进行检测。5种荧光增白剂的质量浓度均在5.0～100mg·L^(-1)内与对应的色谱峰面积呈线性关系,检出限(3S/N)在4～20mg·kg-1之间,测定下限(10S/N)在15～70mg·kg-1之间。对空白样品在5.0,50,100mg·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。

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 10.0mL of acetonitrile(1+2)solution by vortex oscillation for 1min,and then ultrasonically extracted for 10 min.After the mixture was centrifugated at 10 000r·min-1 for 5min,the supernatant was filtered through a 0.22μm filter membrane,and seperated on a MG C18column(250 mm×4.6 mm,5μm),with a mixture of acetonitrile and 10 mmol·L-1 ammonium acetate solution(containing 2mmol·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 5fluorescent whitening agents in the same range of 5.0-100mg·L^-1,with detection limits(3S/N)in the range of 4-20mg·kg-1,and lower limits of determination(10S/N)in the range of 15-70mg·kg-1.Tests for recovery was made to blank samples at mass contentrations of 5.0,50,100mg·L^-1,giving values of recovery between 80.3% and 111%.The 5fluorescent 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%.