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开发一种集超声、离心和超滤于一体的样品预处理装置,将其应用于清热、解毒中成药中非法添加化学成分的快速现场筛选,然后进行电喷雾电离-离子淌度谱分析。

Development of a sample pretreatment device integrating ultrasonication, centrifugation and ultrafiltration, its application on rapid on-site screening of illegally added chemical components in heat-clearing, detoxicating Chinese patent medicines followed by electrospray ionization-ion mobility spectrometry.

机构信息

School of Pharmacy, Hebei Medical University, 361 East Zhongshan Road, Shijiazhuang, 050017, China.

Department of Pharmacy, The Fourth Hospital of Hebei Medical University, Shijiazhuang, 050011, China.

出版信息

J Pharm Biomed Anal. 2021 Feb 5;194:113767. doi: 10.1016/j.jpba.2020.113767. Epub 2020 Nov 20.

DOI:10.1016/j.jpba.2020.113767
PMID:33279301
Abstract

In this paper, a simple and rapid sample pretreatment device integrating ultrasonication, centrifugation and ultrafiltration (UCU) was reported for preparation of trace analytes in complex matrices. The UCU device was composed of two parts, A and B. The sample and extraction solvent were put into Part B for ultrasonic extraction. Subsequently, Part A and Part B were integrated and sealed for centrifugation and ultrafiltration. Finally, the ultrafiltrate in Part A was taken out for subsequent detection. After optimization, the device was applied to rapid on-site screening of five illegally added chemical components in heat-clearing and detoxicating Chinese patent medicines by combining with electrospray ionization-ion mobility spectrometry (ESI-IMS). The method showed good performance in terms of linearity with correlation coefficients (R) above 0.9976 and limits of detection (LODs) in the range of 0.049-0.391 μg mL. The recoveries were from 96.5 % to 100.8 %. The whole analysis process was within 11 min. The proposed method was further compared with other methods reported in the literature and the advantages and considerations were also explored. The results demonstrated that it was a simple, fast and accurate technique. The establishment of this method not only greatly improved the experimental efficiency but also avoided potential sample pollution brought by multiple sample transfer, and could provide a powerful means for rapid on-site analysis of trace analytes in complex matrices.

摘要

本文报道了一种简单快速的样品预处理装置,该装置集成了超声、离心和超滤(UCU),用于制备复杂基质中的痕量分析物。UCU 装置由两部分组成,A 部分和 B 部分。将样品和提取溶剂放入 B 部分进行超声提取。然后,将 A 部分和 B 部分集成并密封进行离心和超滤。最后,从 A 部分取出超滤物进行后续检测。在优化条件下,该装置结合电喷雾电离-离子淌度谱(ESI-IMS)用于快速现场筛选清热解毒中成药中的五种非法添加化学成分。该方法在 0.049-0.391 μg·mL-1 范围内表现出良好的线性性能,相关系数(R)均大于 0.9976,检出限(LOD)较低。回收率在 96.5%至 100.8%之间。整个分析过程在 11 min 内完成。该方法与文献中报道的其他方法进行了比较,并探讨了该方法的优缺点。结果表明,该方法简单、快速、准确。该方法的建立不仅大大提高了实验效率,而且避免了多次样品转移带来的潜在样品污染,为复杂基质中痕量分析物的快速现场分析提供了有力手段。

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