Beale Rachael, Airs Ruth
Plymouth Marine Laboratory, Plymouth, Devon, PL1 3DH, England, United Kingdom.
Anal Chim Acta. 2016 Sep 28;938:114-22. doi: 10.1016/j.aca.2016.07.016. Epub 2016 Jul 25.
A liquid chromatography/mass spectrometry (LC/MS, electrospray ionisation) method has been developed for the quantification of nitrogenous osmolytes (N-osmolytes) in the particulate fraction of natural water samples. Full method validation demonstrates the validity of the method for measuring glycine betaine (GBT), choline and trimethylamine N-oxide (TMAO) in particulates from seawater. Limits of detection were calculated as 3.5, 1.2 and 5.9 pg injected onto column (equivalent to 1.5, 0.6 and 3.9 nmol per litre) for GBT, choline and TMAO respectively. Precision of the method was typically 3% for both GBT and choline and 6% for TMAO. Collection of the particulate fraction of natural samples was achieved via in-line filtration. Resulting chromatography and method sensitivity was assessed and compared for the use of both glass fibre and polycarbonate filters during sample collection. Ion suppression was shown to be a significant cause of reduced instrument response to N-osmolytes and was associated with the presence of seawater in the sample matrix.
已开发出一种液相色谱/质谱联用(LC/MS,电喷雾电离)方法,用于定量天然水样颗粒部分中的含氮渗透物(N-渗透物)。完整的方法验证证明了该方法用于测量海水中颗粒物质中甘氨酸甜菜碱(GBT)、胆碱和氧化三甲胺(TMAO)的有效性。GBT、胆碱和TMAO注入柱中的检测限分别计算为3.5、1.2和5.9皮克(相当于每升1.5、0.6和3.9纳摩尔)。该方法的精密度对于GBT和胆碱通常为3%,对于TMAO为6%。天然样品颗粒部分的收集通过在线过滤实现。在样品收集过程中,评估并比较了使用玻璃纤维和聚碳酸酯过滤器时的色谱结果和方法灵敏度。结果表明,离子抑制是仪器对N-渗透物响应降低的一个重要原因,并且与样品基质中海水的存在有关。