High Flow-Rate Sample Loading in Large Volume Whole Water Organic Trace Analysis Using Positive Pressure and Finely Ground Sand as a SPE-Column In-Line Filter
High Flow-Rate Sample Loading in Large Volume Whole Water Organic Trace Analysis Using Positive Pressure and Finely Ground Sand as a SPE-Column In-Line Filter
复制标题
使用正压和细磨砂作为 SPE 柱在线过滤器，在大容量全水有机痕量分析中进行高流速样品加载
DOI：
10.3390/molecules24071426
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发表时间：
2019
期刊：
影响因子：
4.6
通讯作者：
E. Björklund
中科院分区：
文献类型：
--
作者：
O. Svahn;E. Björklund
通过使用创新的正压进样技术与细砂在线过滤器相结合，可以减少固相萃取 (SPE) 的瓶颈。我们最近发表的工作已经证明了该技术的概念。在这项工作中，重点关注 26 种新兴环境问题化合物的 SPE 流速和方法验证，这些化合物主要来自第一和第二欧盟观察名单，具有各种物理化学性质。在 10、20 和 40 mL/min 三种研究流速下，来自加标纯水样品的研究化合物的平均绝对回收率 (%) 和相对标准偏差 (RSD) (%) 分别为 63.2% (3.2%)、66.9% (3.3%) 和 69.0% (4.0%)。所有三种流速都产生了高度可重复的结果，这使得 200 mg、6 mL 反相 SPE 小柱的流速增加高达 40 mL/min，且不影响回收率。这个数字是制造商推荐的最大流量的四倍多。这表明，当与样品玻璃瓶长时间接触时，某些化合物，尤其是所研究的大环内酯分子，可能会受到影响。减少接触时间可以在一定程度上减少这种并发症。对于使用 40 mL/min 的加标基质丰富池塘水（高浓度和低浓度）和受纳水（河流和废水）进行的实验，也具有非常好的重复性。这项工作表明，对于大量理化性质差异很大的化合物，有一个 10 至 40 mL/min 的宽阔流速窗口，可以进行样品加载。在建议的最大流速 10 mL/min 下，以前需要 50 分钟才能处理 0.5 L 的样品体积，现在使用 40 mL/min 的流速只需 12 分钟即可处理完毕。每个处理样本可节省 38 分钟。这种低成本技术允许样品由取样人员转移到更靠近样品位置的 SPE 柱。这进一步意味着只需将样品盒发送到实验室，而不是像今天的程序那样将整个水样发送到实验室。
By using an innovative, positive pressure sample loading technique in combination with an in-line filter of finely ground sand the bottleneck of solid phase extraction (SPE) can be reduced. Recently published work by us has shown the proof of concept of the technique. In this work, emphasis is put on the SPE flow rate and method validation for 26 compounds of emerging environmental concern, mainly from the 1st and 2nd EU Watch List, with various physicochemical properties. The mean absolute recoveries in % and relative standard deviations (RSD) in % for the investigated compounds from spiked pure water samples at the three investigated flow rates of 10, 20, and 40 mL/min were 63.2% (3.2%), 66.9% (3.3%), and 69.0% (4.0%), respectively. All three flow rates produced highly repeatable results, and this allowed a flow rate increase of up to 40 mL/min for a 200 mg, 6 mL, reversed phase SPE cartridge without compromising the recoveries. This figure is more than four times the maximum flow rate recommended by manufacturers. It was indicated that some compounds, especially pronounced for the investigated macrolide molecules, might suffer when long contact times with the sample glass bottle occurs. A reduced contact time somewhat decreases this complication. A very good repeatability also held true for experiments on both spiked matrix-rich pond water (high and low concentrations) and recipient waters (river and wastewater) applying 40 mL/min. This work has shown that, for a large number of compounds of widely differing physicochemical properties, there is a generous flow rate window from 10 to 40 mL/min where sample loading can be conducted. A sample volume of 0.5 L, which at the recommended maximum flow rate speed of 10 mL/min, would previously take 50 min, can now be processed in 12 min using a flow rate of 40 mL/min. This saves 38 min per processed sample. This low-cost technology allows the sample to be transferred to the SPE-column, closer to the sample location and by the person taking the sample. This further means that only the sample cartridge would need to be sent to the laboratory, instead of the whole water sample, like today’s procedure.