论文部分内容阅读
目的建立测定化妆品中甲萘威的高效液相色谱-柱后衍生测定法。方法水剂、乳状和膏霜状化妆品用甲醇提取后,于5 000 r/min离心,上清液用0.22μm微孔滤膜过滤后,经Carbama Analysis C_8(5μm,4.6 mm×250 mm)色谱柱分离,以水/甲醇=45/55(V/V)为流动相,流速为1.0 ml/min,柱温为37℃,进行分离后,目标物进柱后衍生系统生成高荧光强度的化合物,然后用荧光检测器进行测定,激发波长为330 nm,发射波长为465 nm。结果甲萘威在0.01 mg/L~1.0 mg/L时具有良好的线性,相关系数为0.999 9,方法检出限为0.03 mg/kg,定量限为0.1 mg/kg;在低、中、高3种浓度(0.2 mg/kg、1.0 mg/kg、5.0 mg/kg)添加水平下,回收率为94.9%~103.7%,相对标准偏差为1.16%~5.25%。结论该方法前处理简单,检测灵敏度高,准确度好,适用于水剂、乳状和膏霜状化妆品中甲萘威的测定。
OBJECTIVE To establish a method for the determination of carbaryl in cosmetics by high performance liquid chromatography - post column derivatization. Methods The aqueous, creamy and creamy cosmetics were extracted with methanol and centrifuged at 5000 r / min. The supernatant was filtered through a 0.22 μm microporous membrane and analyzed by Carbama Analysis C_8 (5 μm, 4.6 mm × 250 mm) The column was separated and eluted with a water / methanol = 45/55 (V / V) mobile phase at a flow rate of 1.0 ml / min at a column temperature of 37 ° C to generate a high fluorescence intensity compound , And then measured with a fluorescence detector at an excitation wavelength of 330 nm and an emission wavelength of 465 nm. Results Carbavus had a good linearity in the range of 0.01 mg / L to 1.0 mg / L with a correlation coefficient of 0.999 9. The detection limit was 0.03 mg / kg and the limit of quantification was 0.1 mg / kg. In the low, middle and high The recoveries ranged from 94.9% to 103.7% with relative standard deviations of 1.16% -5.25% at the three concentrations of 0.2 mg / kg, 1.0 mg / kg and 5.0 mg / kg. Conclusion The method is simple, sensitive and accurate. It is suitable for the determination of carbaryl in liquid, creamy and creamy cosmetics.