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Determination of total maleic acid, fumaric acid, p-hydroxybenzoic acid and benzoic acid in food by ultra performance liquid chromatography-tandem mass spectrometry

机译:超高效液相色谱-串联质谱法测定食品中的马来酸,富马酸,对羟基苯甲酸和苯甲酸

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Hydrolysis reaction coupling to ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry (UPLC-MS/MS) was applied for the determination of total maleic acid, fumaric acid, p-hydroxybenzoic acid and benzoic acid in milk-based infant formula, soy-based infant formula, beef jerky, starch and cake. Samples were hydrolyzed by sodium hydroxide and then acidified. The hydrolysis solution was then precipitated by acetonitrile. After being centrifuged, a part of the supernatant was blown dry by nitrogen gas and then dissolved in water for testing. The testing solution was separated by a reverse phase column and then detected by triple quadrupole tandem mass spectrometry operated in a multiple-reaction-monitoring mode. Matrix-matched calibrations were used for quantification. Methyl esters of the acids were used to optimize the influential parameters of the hydrolysis reaction. The matrix effects of the samples on the four acids ranged from 45.7% to 157%. Most of the recoveries at the 50 mg kga?’1 and 200 mg kga?’1 levels were from 74.6% to 129%, with relative standard deviations ranging from 3.5% to 21%. The limits of detection ranged from 1.0 mg kga?’1 to 10.0 mg kga?’1. Fifty samples from the local market were tested.
机译:水解反应与超高效液相色谱-三重四极杆串联质谱(UPLC-MS / MS)联用测定乳基婴儿配方奶粉大豆-中的总马来酸,富马酸,对羟基苯甲酸和苯甲酸基础的婴儿配方食品,牛肉干,淀粉和蛋糕。样品用氢氧化钠水解,然后酸化。然后通过乙腈沉淀水解溶液。离心后,将一部分上清液用氮气吹干,然后溶于水中进行测试。用反相柱分离测试溶液,然后通过在多反应监测模式下运行的三重四极杆串联质谱法进行检测。基质匹配的校准用于定量。酸的甲酯用于优化水解反应的影响参数。样品对四种酸的基质效应范围为45.7%至157%。在50 mg kga-1和200 mg kga-1的水平下,大多数回收率在74.6%至129%之间,相对标准偏差在3.5%至21%之间。检出限为1.0 mg kga?1至10.0 mg kga?1。测试了来自本地市场的50个样品。

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