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磁性碳纳米管的制备及其在生物样品中氰化物代谢产物 2-氨基噻唑啉-4-羧酸的分散微固相萃取中的应用。

Development of magnetic carbon nanotubes for dispersive micro solid phase extraction of the cyanide metabolite, 2-aminothiazoline-4-carboxylic acid, in biological samples.

机构信息

Department of Forensic Science, Sam Houston State University, Huntsville, TX 77341, United States of America.

Department of Chemistry, Sam Houston State University, Huntsville, TX 77341, United States of America.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2019 Mar 1;1109:67-75. doi: 10.1016/j.jchromb.2019.01.020. Epub 2019 Jan 27.

Abstract

2-aminothiazoline-4-carboxylic acid (ATCA) is a minor metabolite of cyanide and is suggested to be a promising biomarker for cyanide exposure due to its specificity to cyanide metabolism and its excellent short- and long-term stability during storage. In this study, magnetic carbon nanotubes, including magnetic multi-walled carbon nanotubes (Mag-MWCNT) and magnetic single-walled carbon nanotubes (Mag-SWCNT) were synthesized as a novel sorbent for dispersive micro solid phase extraction (d-μSPE) to extract ATCA from biological matrices. ATCA spiked deionized water samples with the addition of the isotopic internal standard (ATCA - C, N) were subjected to Mag-CNT/d-μSPE to confirm extraction efficiency of this new technique. The extracted ATCA was derivatized and quantitated using gas chromatography/mass spectrometry (GC/MS) analysis. The extraction parameters were optimized and a detection limits of 15 and 25 ng/mL were obtained for synthetic urine and bovine blood respectively with a linear dynamic range of 30-1000 ng/mL. The optimized Mag-CNT/d-μSPE method facilitated efficient extraction of ATCA using 2 mg of Mag-MWCNT with a 10-minute extraction time. The current assay was also found to be effective for the extraction of ATCA with average recoveries of 97.7 ± 4.0% (n = 9) and 96.5 ± 12.1% (n = 9) from synthetic urine and bovine blood respectively. The approach of using Mag-CNT to facilitate d-μSPE offered a novel alternative to extract ATCA from complex biological matrices.

摘要

2-氨基噻唑啉-4-羧酸(ATCA)是氰化物的一种次要代谢物,由于其对氰化物代谢的特异性和在储存过程中的优异短期和长期稳定性,被认为是氰化物暴露的有前途的生物标志物。在这项研究中,磁性碳纳米管,包括磁性多壁碳纳米管(Mag-MWCNT)和磁性单壁碳纳米管(Mag-SWCNT)被合成作为一种新型的分散固相微萃取(d-μSPE)吸附剂,用于从生物基质中提取 ATCA。向加有同位素内标(ATCA - C,N)的去离子水样品中加入 ATCA 标准品,然后用 Mag-CNT/d-μSPE 进行处理,以验证该新技术的提取效率。提取的 ATCA 经衍生化后,用气相色谱/质谱(GC/MS)分析进行定量。优化了提取参数,在合成尿液和牛血中,分别获得了 15 和 25ng/mL 的检测限,线性动态范围为 30-1000ng/mL。优化后的 Mag-CNT/d-μSPE 方法使用 2mg Mag-MWCNT,10 分钟的提取时间,高效地提取了 ATCA。该方法还被发现对从合成尿液和牛血中提取 ATCA 有效,平均回收率分别为 97.7±4.0%(n=9)和 96.5±12.1%(n=9)。使用 Mag-CNT 促进 d-μSPE 的方法为从复杂的生物基质中提取 ATCA 提供了一种新的选择。

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