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反相离子对超高效液相色谱-质谱联用技术用于指纹分析低分子量肝素。

Reversed-phase ion-pair ultra-high-performance-liquid chromatography-mass spectrometry for fingerprinting low-molecular-weight heparins.

机构信息

Department of Chemistry, University of California - Riverside, Riverside, CA, USA.

出版信息

J Chromatogr A. 2013 May 31;1292:201-10. doi: 10.1016/j.chroma.2013.01.011. Epub 2013 Jan 10.

DOI:10.1016/j.chroma.2013.01.011
PMID:23352830
Abstract

Heparin is a complex mixture of sulfated linear carbohydrate polymers. It is widely used as an antithrombotic drug, though it has been shown to have a myriad of additional biological activities. Heparin is often partially depolymerized in order to decrease the average molecular weight, as it has been shown that low molecular weight heparins (LMWH) possess more desirable pharmacokinetic and pharmacodynamic properties than unfractionated heparin (UFH). Due to the prevalence of LMWHs in the market and the emerging availability of generic LMWH products, it is important that analytical methods be developed to ensure the drug quality. This work explores the use of tributylamine (TrBA), dibutylamine (DBA), and pentylamine (PTA) as ion-pairing reagents in conjunction with acetonitrile and methanol modified mobile phases for reversed-phase ion-pairing ultraperformance liquid chromatography coupled to mass spectrometry (RPIP-UPLC-MS) for fingerprint analysis of LMWH preparations. RPIP-UPLC-MS fingerprints are presented and compared for tinzaparinand enoxaparin.

摘要

肝素是一种复杂的磺酸线性碳水化合物聚合物混合物。它被广泛用作抗血栓药物,尽管已证明它具有许多其他生物活性。肝素通常被部分解聚以降低平均分子量,因为已经证明低分子量肝素(LMWH)比未分级肝素(UFH)具有更理想的药代动力学和药效学特性。由于市场上 LMWHs 的普及以及通用 LMWH 产品的出现,开发分析方法以确保药物质量非常重要。这项工作探讨了使用三丁胺(TrBA)、二丁胺(DBA)和戊胺(PTA)作为与乙腈和甲醇改性流动相一起使用的离子对试剂,用于反相离子对超高效液相色谱与质谱联用(RPIP-UPLC-MS)进行 LMWH 制剂的指纹分析。呈现并比较了tinzaparin 和 enoxaparin 的 RPIP-UPLC-MS 指纹图谱。

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