Quantification of melamine in human urine using cation-exchange based high performance liquid chromatography tandem mass spectrometry
Quantification of melamine in human urine using cation-exchange based high performance liquid chromatography tandem mass spectrometry
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DOI：
10.1016/j.jchromb.2012.01.007
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发表时间：
2012-03-01
影响因子：
3
通讯作者：
Barr, Dana Boyd
中科院分区：
文献类型：
--
作者：
Panuwet, Parinya;Nguyen, Johnny V.;Barr, Dana Boyd
三聚氰胺和三聚氰酸被认为是中国婴儿配方奶粉和北美宠物食品中的掺杂物。在中国，三聚氰胺或三聚氰胺-氰尿酸掺假的影响导致成千上万的中国婴儿肾结石和急性肾衰竭。开发了一种选择性和灵敏的分析方法来测量人体尿液中的三聚氰胺，以评估美国普通人群消费这些类型的掺假产品对健康的潜在影响程度。该方法包括使用阳离子交换固相萃取从人尿液中提取三聚氰胺，使用高效液相色谱在基于二氧化硅的强阳离子交换分析柱上将其与尿液基质共提取物色谱分离，并使用正模式电喷雾电离串联质谱进行分析。使用改良的基于基质的同位素稀释校准进行定量，浓度范围为0.50-100 ng/mL。使用空白和低水平加标样品的重复样品计算的检测限为0.66 ng/mL，相对标准偏差在6.89 - 14.9%之间。三聚氰胺的相对回收率为101- 106%。通过分析从美国一般人群中采集的样本，检测该方法的活力。在76%的测试样本中检测到三聚氰胺，几何平均值为2.37 ng/mL，这表明该方法适用于可靠地检测三聚氰胺或其他可能产生三聚氰胺的化学物质的背景暴露。(c)2012 Elsevier B. V.保留所有权利。
Melamine and cyanuric acid have been implicated as adulterants in baby formula in China and pet foods in North America. In China, the effect of melamine or melamine-cyanuric acid adulteration lead to kidney stone development and acute renal failure in thousands of Chinese infants. A selective and sensitive analytical method was developed to measure melamine in human urine in order to evaluate the extent of potential health implications resulting from the consumption of these types of adulterated products in the general US population. This method involves extracting melamine from human urine using cation-exchange solid-phase extraction, chromatographically separating it from its urinary matrix co-extractants on a silica-based, strong-cation exchange analytical column using high performance liquid chromatography, and analysis using positive mode electrospray ionization tandem mass spectrometry. Quantification was performed using modified, matrix-based isotope dilution calibration covering the concentration range of 0.50-100 ng/mL. The limit of detection, calculated using replicates of blank and low level spiked samples, was 0.66 ng/mL and the relative standard deviations were between 6.89 and 14.9%. The relative recovery of melamine was 101-106%. This method was tested for viability by analyzing samples collected from the general US population. Melamine was detected in 76% of the samples tested, with a geometric mean of 2.37 ng/mL, indicating that this method is suitable for reliably detecting background exposures to melamine or other chemicals from which it can be derived. (c) 2012 Elsevier B.V. All rights reserved.