摘要
采用N,N-二甲基甲酰胺提取样品中的待测物,建立了化妆品中禁、限用着色剂罗丹明B、颜料红57和金光红C的高效液相色谱检测方法。以XDB–Cl8柱为分析柱,5 mmol/L四丁基氢氧化铵–氢氧化钾水溶液(磷酸调至pH 7.00)和甲醇为流动相,梯度洗脱,550 nm(罗丹明B)和480 nm(颜料红57和金光红C)为检测波长,柱温30℃,流速1.0 mL/min,保留时间定性,外标法定量。结果表明在0.25~20 mg/L(罗丹明B和金光红C)、0.5~40mg/L(颜料红57)浓度范围内线性关系良好,检出限分别为5,20,20 mg/kg(S/N=10),实际样品中的加标回收率分别为94.8%~100.5%,95.1%~103.1%,82.5%~90.5%,相对标准偏差为0.9%~4.6%。该方法前处理简单、易操作,检测结果准确可靠,能够满足化妆品中这3种着色剂的检测要求和监管需要。
The cosmetic samples were extracted by DMF, a quantitative detection method for determination of Rhodamine B, Lake Red C and Pigment Red 57, which were forbidden or limited to be used in cosmetics was established by high performance liquid chromatography with diode array detector. The target compounds were separated on a XDB-C18 column in gradient elution mode using 5 mmol/L tetrabutylammonium hydroxide and KOH aqueous solution (pH 7.00, adjusted by phosphoric acid) and methanol as mobile phase. The detective wavelength was 550 nm for Rhodamine B and 480 mn for Pigment Red 57 and Lake Red C, and the colunm temperature was 30℃ while the flow rate of the mobile phase was 1.0 mL /min. Under the optimal chromatographic conditions, the three colorants were analyzed qualitatively based on its retention time while the quantitative analysis was carried out by external standard method. The calibration plot of peak area versus concentration showed good linearity between 0.25 and 20.0 mg/L for Rhodamine B and Lake Red C, 0.5-40.0 mg / L for Pigment Red 57, the correlation coefficients were more than 0.999 9, the detection limits and recoveries of Rhodamine B, Lake Red C and Pigment Red 57 were 5,20,20 mg/kg ( S/N=IO ) and 94.8%-100.5%, 95.1%-103.1%, 82.5%-90.5%, respectively. The relative standard deviation was 0.9%-4.6%. The results indicated that the developed method is sample, rapid, accurate and suitable for the detection of three colorants in cosmetics samples and requirements of supervision.
出处
《化学分析计量》
CAS
2012年第6期36-39,共4页
Chemical Analysis And Meterage