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Unbiased Measurement of Phosphate and Phosphorus Speciation in Surface Waters

机译：地表水中磷酸盐和磷形态的无偏测量

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摘要

Trace-level phosphate analysis and phosphorus speciation in surface water remained challenging due to adsorption and phosphate uptake by microorganisms. In this study a two-dimensional ion chromatography separation coupled to electrospray ionization high-resolution mass spectrometry (2D-IC-ESI-MS) allowed isotope dilution quantitation of phosphate with simultaneous analysis of 11 phosphate-containing metabolites and two inorganic condensed phosphates. Samples were collected from Lake St. Clair, Lake Ontario, and Georgian Bay (ON, Canada). Comparative experiments showed lower phosphate results for samples not immediately spiked and for external calibration quantitation. Field spiking with O-18-labeled phosphate combined with isotope dilution quantitation allows measurement of the phosphate levels existent at the collection time instead of the phosphate concentrations remaining in the samples at the analysis time. This is a significant advantage against the traditional colorimetric and ion chromatographic (IC) analysis methods, which are unable to compensate for the adsorption loss occurring in standards and samples, especially when phosphate is present at levels below 20 mu g L-1 as P (61 mu g L-1 as PO43-). Two phosphate-containing metabolites, adenosine 5'-monophosphate (AMP) and D-glucose 6-phosphate (Glucose-P), were detected in a subset of samples collected from Lake St. Clair, with no statistically significant correlation between them and the simultaneously measured phosphate. Directly bioavailable P (phosphate), indirectly bioavailable P (phosphatase-hydrolyzed P) and nonbioavailable P (nonhydrolizable P) fractions were quantified by measuring phosphate, phosphate after phosphatase addition and total phosphorus. The proposed 2D-IC-ESI-MS method developed for a QExactive MS instrument with field spiking of the internal standard provides accurate phosphate results and eliminates quantitation errors caused by phosphate adsorption. This setup allows simultaneous collection of targeted and nontargeted analysis data and thus the detection of trace polar organic phosphorus metabolites as well.
机译：由于微生物的吸附和磷酸盐吸收，地表水中的痕量磷酸盐分析和磷形态仍然具有挑战性。在这项研究中，二维离子色谱分离与电喷雾电离高分辨率质谱（2D-IC-ESI-MS）结合使用，可同时分析11种含磷酸盐的代谢物和两种无机缩合磷酸盐，从而对磷酸盐进行同位素稀释定量。样品采集自圣克莱尔湖，安大略湖和乔治亚湾（加拿大安大略省）。对比实验表明，对于未立即加标的样品和外部校准定量，磷酸盐结果较低。 O-18标记的磷酸盐与同位素稀释定量相结合的现场加标可以测量收集时存在的磷酸盐水平，而不是分析时样品中残留的磷酸盐浓度。与传统的比色和离子色谱（IC）分析方法相比，这是一个重要优势，传统的比色和离子色谱（IC）分析方法无法补偿标准品和样品中发生的吸附损失，尤其是当磷酸盐的含量低于20μg L-1时，P（ 61μgL-1为PO43-）。在从圣克莱尔湖收集的一部分样品中检测到两种含磷酸盐的代谢物，腺苷5'-单磷酸盐（AMP）和D-葡萄糖6-磷酸盐（Glucose-P），与它们之间没有统计学意义的相关性。同时测量磷酸盐。通过测量磷酸盐，添加磷酸酶后的磷酸盐和总磷来定量直接可生物利用的P（磷酸盐），间接可生物利用的P（磷酸酶水解的P）和不可生物利用的P（不可水解的P）部分。为QExactive MS仪器开发的拟议的2D-IC-ESI-MS方法具有内标的现场加标，可提供准确的磷酸盐结果，并消除了由磷酸盐吸附引起的定量误差。此设置允许同时收集目标分析和非目标分析数据，因此也可以检测痕量极性有机磷代谢物。

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  • 来源
    《Environmental Science & Technology》 |2019年第2期|820-828|共9页
  • 作者

    Packa Vlastimil; Maedler Stefanie; Howell Todd; Bostan Vadim; Diep Ngan; Tooley Robert; Furdui Vasile I.;

  • 作者单位

    Ontario Minist Environm Conservat & Pk, 125 Resources Rd, Toronto, ON M9P 3V6, Canada|Ryerson Univ, 350 Victoria St, Toronto, ON M5B 2K3, Canada;

    Ontario Minist Environm Conservat & Pk, 125 Resources Rd, Toronto, ON M9P 3V6, Canada;

    Ontario Minist Environm Conservat & Pk, 125 Resources Rd, Toronto, ON M9P 3V6, Canada;

    Ryerson Univ, 350 Victoria St, Toronto, ON M5B 2K3, Canada;

    Ontario Minist Environm Conservat & Pk, 125 Resources Rd, Toronto, ON M9P 3V6, Canada;

    Ontario Minist Environm Conservat & Pk, 125 Resources Rd, Toronto, ON M9P 3V6, Canada;

    Ontario Minist Environm Conservat & Pk, 125 Resources Rd, Toronto, ON M9P 3V6, Canada|Ryerson Univ, 350 Victoria St, Toronto, ON M5B 2K3, Canada;

  • 收录信息 美国《科学引文索引》(SCI);美国《工程索引》(EI);美国《生物学医学文摘》(MEDLINE);美国《化学文摘》(CA);
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