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Fast and sensitive determination of 10 forbidden phthalates in perfumes by ultra-high performance liquid chromatography-electrospray ionization-tandem mass spectrometry

机译:通过超高效液相色谱 - 电喷雾电离 - 串联质谱法快速敏感地测定10种禁止的邻苯二甲酸盐。

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A fast and sensitive ultra-high performance liquid chromatography-electrospray ionization-tandem mass spectrometry (UHPLC-ESI-MS/MS) method was developed for simultaneously analyzing 10 phthalates in perfume, which are forbidden by the hygienic standards for cosmetics in China (2007 edition). Matrix effect is significant on a phthalate when it is co-eluted with other phthalates. Improving the resolution between adjacent phthalate peaks is found effective in reducing the matrix effects. Thus, simultaneous analysis of the 10 phthalates requires successful resolutions of each phthalate. Nonetheless, a trade-off between the resolution and analysis time results either incomplete separation or prolonged analysis time. Here, the UHPLC elution gradient is optimized considering the predicted retention time of each phthalate. The resolutions and matrix effects of targeted compounds are evaluated to determine the optimal elution gradient for UHPLC-MS analysis method. Under the optimized gradient, the resolution between closest phthalate peaks is beyond 1.7, while the analysis time is merely 7 min. Except for dimethyl phthalate (DMP) and dicyclohexyl phthalate (DCHP), insignificant matrix effects have been found on all the phthalates. Direct quantifications through external calibration curve are appropriate for such analytes. Nonetheless, DMP and DCHP suffering obvious matrix effects require extra analyses of spiked samples for the quantifications through the standard addition method. Instrumental limits of quantitation (iLOQs) are 0.12-89 mu g L-1 for the targeted phthalates. Meanwhile, the accuracy and precision of the analytical method are good. Finally, the forbidden phthalates in 26 sampled perfumes are successfully analyzed by the developed method. (C) 2018 Elsevier B.V. All rights reserved.
机译:开发了一种快速敏感的超高效液相色谱 - 电喷雾电离 - 串联质谱(UHPLC-ESI-MS / MS)方法,同时分析了香料中的10个邻苯二甲酸盐,这是由中国化妆品的卫生标准禁止(2007年版)。当用其他邻苯二甲酸盐共同洗脱时,基质效应在邻苯二甲酸酯上显着。提高相邻邻苯二甲酸盐峰之间的分辨率被发现有效降低基质效应。因此,对10个邻苯二甲酸酯的同时分析需要每种邻苯二甲酸酯的成功分辨率。尽管如此,分辨率与分析时间之间的权衡导致分离或长时间分析时间不完整。这里,考虑到每种邻苯二甲酸盐的预测保留时间来优化UHPLC洗脱梯度。评价靶向化合物的分辨率和基质效应以确定UHPLC-MS分析方法的最佳洗脱梯度。在优化的梯度下,最近邻苯二甲酸盐之间的分辨率超过1.7,而分析时间仅仅是7分钟。除邻苯二甲酸二甲酯(DMP)和邻苯二甲酸二环己酯(DCHP)外,在所有邻苯二甲酸盐上发现了不显着的基质效应。通过外部校准曲线直接定量适用于这种分析物。尽管如此,DMP和DCHP患有明显的基质效应需要通过标准添加方法进行尖刺样品的额外分析。靶向邻苯二甲酸盐的仪器定量限制(ILOQ)为0.12-89μgl-1。同时,分析方法的准确性和精度良好。最后,通过开发的方法成功分析了26个采样香料中的禁止邻苯二甲酸酯。 (c)2018年elestvier b.v.保留所有权利。

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