超高效液相色谱法检测化妆品中的12种磺胺抗生素

Determination of 12 Sulfonamides in Cosmetics by Ultra Performance Liquid Chromatography

建立了采用超高效液相色谱(UPLC)-二极管阵列检测器(PDA)测定化妆品中12种常见的磺胺抗生素(磺胺、磺胺间甲氧嘧啶、磺胺醋酰、磺胺甲基异唑、磺胺嘧啶、磺胺二甲异唑、磺胺噻唑、磺胺二甲氧嘧啶、磺胺甲基嘧啶、磺胺喹啉、磺胺二甲嘧啶、磺胺硝苯)的方法。采用Acquity UPLCTMBEHC C18色谱柱(50mm×2.1mm,1.7μm),流动相为乙腈/0.1%的甲酸水溶液,梯度洗脱。样品经提取、反萃取后,用UPLC-PDA进行分析检测,结合保留时间和紫外光谱进行定性分析,定量检测波长268nm。12种磺胺的检出限(S/N=3)均为1μg/g,定量下限(S/N=10)为2-3μg/g,在1-25mg/L(磺胺硝苯为0.5-12.5mg/L)范围内,峰面积和质量浓度的线性关系良好(r>0.999 7)。添加水平为40,8μg(磺胺硝苯为20,4μg)时,12种磺胺的平均回收率分别为86.8%-98.1%和80.1%-96.9%,相对标准偏差小于10%(n=6)。结果表明该方法简单,分离效果好,速度快,能够满足检测化妆品中12种常见的磺胺抗生素的需要。

A method for the determination of 12 sulfonamides （SAs） （sulfanilamide, sulfamonomethoxine, sulfacetamide, sulfamethoxazole, sulfadiazine, sulfisoxazole, sulfathiazole, sulfadimethoxine, sulfamerazine, sulfaquinoxaline, sulfamethazine, sulfanitran） in cosmetics was developed by ultra performance liquid chromatography with photodiode array detector （UPLC- PDA）. The chromatographic column used was Acquity UPLCTM BEHC C18 （50 mm × 2. 1 mm, 1.7 μm） and the mobile phase was acetonitrile-0. 1% formic acid aqueous solution. A gradient elution program was utilized for the separation and determination. After liquid-liquid extraction, SAs were separated and detected by UPLC-PDA. The qualification analysis was done by using retention time and spectrum, and the quantification was based on the detection wavelength of 268 nm. The limits of qualification （S/N=3） and quantification （S/N= 10） for 12 SAs were 1 p.g/g and 2 -3 μg/g, respectively. The correlation coefficient of linear calibration curve was over 0. 999 7 within the SAs concentration range of 1 -25 mg/L （ except sulfanitran 0. 5 - 12.5 mg/L）. At the spiked levels of 40 and 8 μg（except suifauitran 20 and 4μg）, the average recoveries for 12 SAs were 86. 8% -98. 1% and 80. 1% -96. 9%, respectively. Relative standard deviations were less than 10%. Routine tests show that the method is simple, fast, and has a good separation efficiency. It can be routinely used for the determination of these SAs in cosmetics.