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UPLC-ESI-MS/MS method for the quantitative measurement of aliphatic diamines, trimethylamine N-oxide, and β-methylamino-l-alanine in human urine
Journal of Chromatography B ( IF 3 ) Pub Date : 2018-03-02 , DOI: 10.1016/j.jchromb.2018.02.043
Deepak Bhandari , Brett A. Bowman , Anish B. Patel , David M. Chambers , Víctor R. De Jesús , Benjamin C. Blount

This work describes a quantitative high-throughput analytical method for the simultaneous measurement of small aliphatic nitrogenous biomarkers, i.e., 1,6-hexamethylenediamine (HDA), isophoronediamine (IPDA), β-methylamino-l-alanine (BMAA), and trimethylamine N-oxide (TMAO), in human urine. Urinary aliphatic diamines, HDA and IPDA, are potential biomarkers of environmental exposure to their corresponding diisocyanates. Urinary BMAA forms as a result of human exposure to blue-green algae contaminated food. And, TMAO is excreted in urine due to the consumption of carnitine- and choline-rich diets. These urinary biomarkers represent classes of small aliphatic nitrogen-containing compounds (N-compounds) that have a high aqueous solubility, low logP, and/or high basic pKa. Because of the highly polar characteristics, analysis of these compounds in complex sample matrices is often challenging. We report on the development of ion-pairing chemistry based ultra-performance liquid chromatography–electrospray ionization–tandem mass spectrometry (UPLC–ESI–MS/MS) method for the simultaneous measurement of these biomarkers in human urine. Chromatographic separation was optimized using heptafluorobutyric acid-(HFBA-) based mobile phase and a reversed-phase C18 column. All four analytes were baseline separated within 2.6 min with an overall run time of 5 min per sample injection. Sample preparation involved 4 h of acid hydrolysis followed by automated solid phase extraction (SPE) performed using strong cation exchange sorbent bed with 7 N ammonia solution in methanol as eluent. Limits of detection ranged from 0.05 ng/mL to 1.60 ng/mL. The inter-day and intra-day accuracy were within 10%, and reproducibility within 15%. The method is accurate, fast, and well-suited for biomonitoring studies within targeted groups, as well as larger population-based studies such as the U. S. National Health and Nutrition Examination Survey (NHANES).



中文翻译:

UPLC-ESI-MS / MS方法定量测定人尿中的脂肪族二胺,三甲胺N-氧化物和β-甲基氨基-1-丙氨酸

这项工作描述了一种定量的高通量分析方法,用于同时测量小的脂肪族含氮生物标志物,即1,6-六亚甲基二胺(HDA),异佛尔酮二胺(IPDA),β-甲基氨基-1-丙氨酸(BMAA)和三甲胺N尿中的氧化铁(TMAO)。尿脂族二胺,HDA和IPDA是环境暴露于其相应的二异氰酸酯的潜在生物标志物。尿液BMAA的形成是人类暴露于蓝藻污染的食物的结果。而且,由于食用富含肉碱和胆碱的饮食,TMAO会在尿液中排泄。这些尿液生物标志物代表水溶性高,对数P低的小型脂肪族含氮化合物(N-化合物)和/或较高的基本p K a。由于具有极高的极性,因此在复杂的样品基质中分析这些化合物通常具有挑战性。我们报告了基于离子对化学的超高效液相色谱-电喷雾电离-串联质谱法(UPLC-ESI-MS / MS)的发展,用于同时测量人尿液中的这些生物标志物。色谱分离使用基于七氟丁酸-(HFBA-)的流动相和反相C18色谱柱进行了优化。在2.6分钟内将所有四种分析物进行基线分离,每次进样的总运行时间为5分钟。样品制备涉及4小时的酸水解,然后使用强阳离子交换吸附剂床和7 N氨在甲醇中的溶液作为洗脱剂进行自动固相萃取(SPE)。检测限范围从0.05 ng / mL到1。60 ng / mL。日间和日内准确性在10%以内,重现性在15%以内。该方法准确,快速并且非常适合目标群体内的生物监测研究,以及以人群为基础的研究,例如美国国家健康与营养调查(NHANES)。

更新日期:2018-03-02
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