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Rapid Determination of 10 Parabens in Spices by High Performance Liquid Chromatography- Mass Spectrometry

机译:高效液相色谱-质谱法快速测定香料中的十种对羟基苯甲酸酯

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An ultra-high-performance liquid chromatography with electrospray ionization tandem mass spectrometry (UHPLC-ESI-MS/MS) method was developed for determination of ten parabens (methyl-, ethyl-, propyl-, isopropyl-, butyl-, isobutyl-, amyl-, isoamyl-, hexyl-, and heptyl-parabens) in spices. After simple preparation, the extract was injected directly into the UHPLC-MS/MS system. Parabens were separated on an Acquity UPLC BEH C18 column using gradient elution programming and detected by the tandem quadrupole mass spectrometer operating in a negative-ion electrospray-ionization (-ESI) mode. The total run time of liquid chromatography was 13 min. Linear calibration curves of 10 parabens were obtained in the range of 0.10-20.00 ng/mL under optimum conditions (r > 0.9990). The limits of detection (LOD) and the limits of quantification (LOQ) were in the range between 0.01-0.08 ng/g and 0.03-0.20 ng/g, respectively. Intra-day precision and inter-day precision were 1.04%-2.13% and 1.03%-3.16%, respectively. Recoveries were between 89.41% and 99.30%. This proposed method was successfully applied in 11 kinds of spices (38 brands). In these samples, combinations of parabens appeared more frequently than we anticipated, and 63.16% of them contained more than one paraben. As a result, it was necessary to simultaneously test for 10 parabens in spices.
机译:开发了一种采用电喷雾电离串联质谱(UHPLC-ESI-MS / MS)的超高效液相色谱法,用于测定十种对羟基苯甲酸酯(甲基,乙基,丙基,异丙基,丁基,异丁基,香料中的戊基,戊基,戊基,戊基,戊基)简单制备后,将提取物直接注入UHPLC-MS / MS系统。使用梯度洗脱程序在Acquity UPLC BEH C18色谱柱上分离对羟基苯甲酸酯,并通过串联四极杆质谱仪在负离子电喷雾电离(-ESI)模式下进行检测。液相色谱仪的总运行时间为13分钟。在最佳条件下(r> 0.9990),在0.10-20.00 ng / mL范围内获得了10种对羟基苯甲酸酯的线性校准曲线。检测限(LOD)和定量限(LOQ)分别在0.01-0.08 ng / g和0.03-0.20 ng / g之间。日内精度和日间精度分别为1.04%-2.13%和1.03%-3.16%。回收率介于89.41%和99.30%之间。该方法成功应用于11种香料(38个品牌)。在这些样品中,对羟基苯甲酸酯的组合出现的频率比我们预期的要高,其中63.16%包含不止一种对羟基苯甲酸酯。结果,有必要同时测试香料中的10种对羟基苯甲酸酯。

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