高效液相色谱荧光法测定化妆品中的10种荧光着色剂

Determination of 10 fluorescent colorants in cosmetics by high performance liquid chromatography with fluorescence detection

建立了一种同时测定化妆品中10种荧光着色剂(荧光素、荧光素钠、二溴荧光素、二碘荧光素、二碘荧光素二钠、四溴荧光素、四溴荧光素二钠、四溴四氯荧光素、四氯四溴荧光素二钠、罗丹明B)的高效液相色谱-荧光检测方法,并用该方法对眉笔、口红、眼影、腮红等30多个产品进行了检测。样品经提取过滤后,以10 mmol/L甘氨酸-甲醇为流动相,用Waters XBridge C_(18)(5μm×4.6 mm×250 mm)色谱柱分离,高效液相色谱-荧光检测器进行定性和定量分析。结果表明,10种荧光着色剂的质量浓度与峰面积之间呈良好线性关系(R2>0.998)。二碘荧光素/二碘荧光素二钠的检出限为1μg/g,定量限为3μg/g,其余荧光着色剂的检出限为0.2μg/g,定量限为0.5μg/g。在高、中、低3种加标水平下,各目标化合物的回收率为88.7%~118.5%,相对标准偏差为1.8%~8.2%(n=6)。该方法前处理简便快捷、灵敏度高、基质干扰小,适用于化妆品中10种荧光着色剂的同时检测。

A method for the simultaneous determination of 10 fluorescent colorants(fluorescein,sodium fluorescein,dibromofluorescein,diiodofluorescein,disodium diiodofluorescein,tetrabromofluorescein,disodium tetrabromofluorescein,tetrachlorotetrabromofluorescein,disodium tetrachloro-tetrabromofluorescein and rhodamine B)in cosmetics by high performance liquid chromatography with fluorescence detection was established.This method was used to monitor the risk for more than 30 products including eyebrow pencils,lipsticks,eye shadows and blushers.The effects of extraction solvents on the fluorescent colorants were explored,and it is found that when the extraction solvent is methanol,the recovery rate of various fluorescent colorants can reach the best level.Meanwhile,to obtain higher sensitivity,the alkaline mobile phase glycine-methanol system was used to separate the fluorescent colorants.The effects of pH and concentration of glycine buffer solutions on the resolution and fluorescence intensity of the ten fluorescent colorants were also studied.It is found that when the pH is 9.0 and the concentration is 10 mmol/L,the resolution and fluorescence intensity of the 10 fluorescent colorants can achieve the best results.Finally,the fluorescent colorants were separated by Waters XBridge C_(18)(5μm×4.6 mm×250 mm)column using 10 mmol/L glycine-methanol as the mobile phase,and qualitative and quantitative analysis was performed by high performance liquid chromatography with a fluorescence detector.The results show that there is a good linear relationship between concentration and peak area with R2 no less than 0.998.The limits of detection for diiodofluorescein and disodium diiodofluorescein are 1μg/g and the limits of quantification are 3μg/g,while the limits of detection for other fluorescent colorants are 0.2μg/g and the limits of quantification are 0.5μg/g.The average recoveries are from 88.7%to 118.5%,with relative standard deviations are in the range of 1.8%-8.2%(n=6).This method has advantages such as simple pretreatment,high sensitivity and almost little interference from matrix.It is suitable for the simultaneous determination of the 10 fluorescent colorants in cosmetics.The method is expected to fill the gap in current detection methods and provide strong technical support for the quality monitoring and residue analysis of fluorescent colorants in cosmetics.