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Determination of formaldehyde residue in cosmetics by short-column high performance liquid chromatography with mass spectrometric confirmation

机译:短柱高效液相色谱法测定化妆品中甲醛残留物,质谱鉴定

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In this work, we report a rapid analytical method for the determination of trace formaldehyde in cosmetics on a 12.5 mm C18 guard column. The shortest time (0.5 min) was obtained for one separation with 1.5 mL mina?’1 of methanola€“water 50:50 (v/v) as the mobile phase at a column temperature of 30 ?°C. A linear response between peak area and the concentration of formaldehyde was obtained over the range 0.1 to 20 mg La?’1 with a relative standard deviation of 1.4% (n = 10) at the concentration of 1.0 mg La?’1 and a detection limit of 5.1 ??g La?’1. The confirmation assay by liquid chromatography tandem mass spectrometry indicated that there was no interfering effect from other carbonyl compounds. The proposed method was applied for the determination of formaldehyde residue in cosmetics at the mg La?’1 level. Free formaldehyde up to 27 mg kga?’1 was found in cosmetics and the spike recovery at the spiked levels of 1.0 and 10.0 mg La?’1 varying from 92% to 105% was also obtained. The difference between the values determined by the proposed method and the standard spectrophotometric method was below 3.7%. The results proved the accuracy and precision of the method, showing potential for the routine analysis of formaldehyde residue.
机译:在这项工作中,我们报告了一种快速分析方法,用于测定12.5 mm C18保护柱的化妆品中痕量甲醛。获得最短的时间(0.5分钟),得到1.5mL MINA的一个分离,其中甲醇蛋白为50:50(v / v),为30Ω·℃的柱温下的流动相。在0.1至20mg的La = 1的范围内获得峰面积和甲醛浓度之间的线性响应,其相对标准偏差为1.4%(n = 10),浓度为1.0mg la-1和检测限制5.1 ?? g la?'1。通过液相色谱法串联质谱法的确认测定表明,没有来自其他羰基化合物的干扰效果。所提出的方法用于测定Mg La-1水平的化妆品中的甲醛残留物。在化妆品中发现免费甲醛,高达27毫克kga?1中发现了1.0和10.0 mg la的尖峰水平的尖峰恢复,也得到了92%至105%的0.5%。所提出的方法和标准分光光度法确定的值与标准分光光度法之间的差异低于3.7%。结果证明了该方法的准确性和精度,显示了甲醛残留的常规分析的潜力。

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