Zheng Hehui, Wang Ping, Li Jie
Beijing Center for Disease Prevention and Control, Beijing 100013, China.
Se Pu. 2007 Mar;25(2):238-40.
A method for the determination of 12 sulfonamides (SAs) (sulfanilamide, sulfamonomethoxine, sulfacetamide, sulfamethoxazole, sulfadiazine, sulfisoxazole, sulfathiazole, sulfadi-methoxine, 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 UPLC BEHC C18 (50 mm x 2. 1 mm, 1. 7 microm) 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 microg/g and 2 -3 microg/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 microg (except sulfanitran 20 and 4 microg), 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.
建立了一种采用超高效液相色谱-光电二极管阵列检测器（UPLC-PDA）测定化妆品中12种磺胺类药物（SAs）（磺胺、磺胺间甲氧嘧啶、磺胺醋酰、磺胺甲恶唑、磺胺嘧啶、磺胺异恶唑、磺胺噻唑、磺胺二甲氧嘧啶、磺胺甲基嘧啶、磺胺喹恶啉、磺胺二甲嘧啶、磺胺硝苯）的方法。所用色谱柱为Acquity UPLC BEHC C18（50 mm×2.1 mm，1.7 µm），流动相为乙腈-0.1%甲酸水溶液。采用梯度洗脱程序进行分离测定。经液-液萃取后，用UPLC-PDA对SAs进行分离检测。通过保留时间和光谱进行定性分析，定量基于268 nm的检测波长。12种SAs的定性限（S/N = 3）和定量限（S/N = 10）分别为1 μg/g和2 - 3 μg/g。在1 - 25 mg/L的SAs浓度范围内（磺胺硝苯为0.5 - 12.5 mg/L），线性校准曲线的相关系数均大于0.999 7。在40和8 μg的加标水平下（磺胺硝苯为20和4 μg），12种SAs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%。常规试验表明，该方法简便、快速，分离效率良好。可常规用于化妆品中这些SAs的测定。
