超高效液相色谱法测定口腔护理产品中异噻唑啉酮类含量

Determination of thiazolidinones in oral care products by ultra performance liquid chromatography

采用超高效液相色谱法测定口腔护理产品中异噻唑啉酮类含量。通过HyperSep反相C8/苯磺酸离子交换器(HyperSep C8/BSAIE),Sep-Pak C18吸附剂的固相萃取(SPE)及超高效液相色谱/二极管阵列检测器(UPLC/DAD)用于同时测定口腔护理产品中甲基异噻唑啉酮(MI)和甲基氯异噻唑啉酮(MCI)。结果发现,HyperSep C8/BSAIE和UPLC/DAD的洗脱溶剂为混合物(乙腈和甲醇体积比2∶1),较佳检测波长为255 nm;该方法具有良好的线性范围(0.005~10μg/mL),测定系数(R^(2),0.997~0.999),检测限(LOD,0.001~0.002μg/g);在检测低(0.07μg/mL)、中(3μg/mL)和高(15μg/mL)质量浓度的标准混合物时,相对标准偏差RSD<3%。共研究了12个口腔护理样品,MI含量为nd~0.89μg/g,MCI含量为nd~0.62μg/g。根据样品的类型,回收率在95.33%~101.43%之间。

The purpose of this paper is to determine the content of isothiazolinones in oral care products by ultra performance liquid chromatography.A HyperSep reversed-phase C8/BSAIE ion exchanger,solid phase extraction(SPE)with Sep-Pak C18 sorbent and an ultra performance liquid chromatography/diode array detector(UPLC/DAD)were used for the simultaneous determination of methylisothiazolinone(MI)and methylchloroisothiazolinone(MCI)in oral care products.The results find that the eluting solvents for HyperSep C8/BSAIE and UPLC/DAD are mixtures(acetonitrile/methanol,volume ratio 2∶1)with an optimum detection wavelength of 255 nm.The method has a good linear range(0.005-10μg/mL),the coefficient of determination(R^(2))ranges from 0.997 to 0.999,and the limit of detection(LOD)is in the range of 0.001-0.002μg/g.The relative standard deviation RSD is less than 3%for the detection of standard mixtures at low(0.07μg/mL),medium(3μg/mL)and high(15μg/mL)concentrations.A total of 12 oral care samples are studied,with the reaching concentrations of nd-0.89μg/g for MI and nd-0.62μg/g for MCI.Recoveries range from 95.33%to 101.43%depending on the type of sample.