Department of Pharmacy, Center for Drug Research, Ludwig-Maximilians-Universität München, 81377 Munich, Germany.
Molecules. 2024 Sep 30;29(19):4656. doi: 10.3390/molecules29194656.
Dispersive solid-phase extraction (dSPE) is a crucial step for multiresidue analysis used to remove matrix components from extracts. This purification prevents contamination of instrumental equipment and improves method selectivity, sensitivity, and reproducibility. Therefore, a clean-up step is recommended, but an over-purified extract can lead to analyte loss due to adsorption to the sorbent. This study provides a systematic comparison of the advantages and disadvantages of the well-established dSPE sorbents PSA, GCB, and C18 and the novel dSPE sorbents chitin, chitosan, multi-walled carbon nanotube (MWCNT), and Z-Sep (zirconium-based sorbent). They were tested regarding their clean-up capacity by visual inspection, UV, and GC-MS measurements. The recovery rates of 98 analytes, including pesticides, active pharmaceutical ingredients, and emerging environmental pollutants with a broad range of physicochemical properties, were determined by GC-MS/MS. Experiments were performed with five different matrices, commonly used in food analysis (spinach, orange, avocado, salmon, and bovine liver). Overall, Z-Sep was the best sorbent regarding clean-up capacity, reducing matrix components to the greatest extent with a median of 50% in UV and GC-MS measurements, while MWCNTs had the largest impact on analyte recovery, with 14 analytes showing recoveries below 70%. PSA showed the best performance overall.
分散固相萃取（dSPE）是多残留分析中用于从提取物中去除基质成分的关键步骤。这种净化可以防止仪器设备的污染，并提高方法的选择性、灵敏度和重现性。因此，推荐进行净化步骤，但如果过度净化提取物，由于吸附到吸附剂上，可能会导致分析物损失。本研究系统比较了 PSA、GCB 和 C18 等成熟的 dSPE 吸附剂以及甲壳素、壳聚糖、多壁碳纳米管（MWCNT）和 Z-Sep（基于锆的吸附剂）等新型 dSPE 吸附剂的优缺点。通过目视检查、UV 和 GC-MS 测量来测试它们的净化能力。通过 GC-MS/MS 测定了 98 种分析物（包括农药、活性药物成分和具有广泛物理化学性质的新兴环境污染物）的回收率。实验使用了五种不同的基质，常用于食品分析（菠菜、橙子、鳄梨、三文鱼和牛肝）。总体而言，Z-Sep 在净化能力方面表现最好，在 UV 和 GC-MS 测量中，将基质成分最大程度地降低至中位数 50%，而 MWCNTs 对分析物回收率的影响最大，有 14 种分析物的回收率低于 70%。PSA 的整体性能最好。
