Fresenius Kabi AB, SE-196 37 Kungsängen, Sweden.
J Chromatogr B Analyt Technol Biomed Life Sci. 2010 Oct 1;878(27):2497-501. doi: 10.1016/j.jchromb.2010.02.012. Epub 2010 Feb 16.
A molecularly imprinted polymer, MIP, was prepared and evaluated as SPE sorbent for a cyclicized adduct formed to N-terminal valine (Pyr-Val) in hemoglobin from 1,2:3,4-diepoxybutane (DEB). This metabolite plays an important role in the carcinogenesis of 1,3-butadiene. The hydrazide of Pyr-Val, formed after hydrazinolysis of hemoglobin, as well as necessary standards was synthesized. The MIP was prepared from methacrylic acid with a structure analogue to the investigated adduct as template and the method was developed for aqueous conditions. Selective desorption was achieved when the sample was washed with water after loading in 10% acetonitrile. The primary interaction with the binding sites in the imprints was most likely of ionic character. Quantification of the Pyr-Val adduct was performed with LC/ESI-MS/MS, yielding an instrumental LOD of 150 pg injected amount.
制备了一种分子印迹聚合物（MIP），并将其评估为 SPE 吸附剂，用于从 1,2:3,4-二环氧丁烷（DEB）中血红蛋白的 N-末端缬氨酸（Pyr-Val）形成的环状加合物。这种代谢物在 1,3-丁二烯的致癌作用中起着重要作用。Pyr-Val 的酰肼，在血红蛋白的肼解后形成，以及必要的标准品被合成。MIP 是由甲基丙烯酸制备的，其结构类似于研究中的加合物作为模板，并在水相条件下开发了该方法。在 10％乙腈中加载后，用水洗去样品时，实现了选择性洗脱。与印迹中的结合位点的主要相互作用可能具有离子特性。用 LC/ESI-MS/MS 对 Pyr-Val 加合物进行定量，得到仪器检测限为 150 pg 进样量。
