公开(公告)号：US20150087073A1

公开(公告)日：2015-03-26

申请号：US14394952

申请日：2013-03-14

Applicant: Waters Technologies Corporation

Inventor： Erin E. Chambers ,  Martha Stapels ,  Joanne Mather

IPC: G01N33/74

CPC classification number: G01N33/6848 ,  G01N30/7233 ,  G01N30/7266 ,  G01N30/8679 ,  G01N30/88 ,  G01N33/02 ,  G01N33/74 ,  G01N2030/8831 ,  Y10T436/24

Abstract: A method for identifying a polypeptide a specimen can include (i) treating a specimen suspected of comprising an insulin with a base; (ii) extracting a first fraction of the treated specimen by solid phase extraction using a mixed mode or polymeric reversed-phase media and a first solvent comprising an acid; (iii) separating a component of the first fraction by liquid chromatography using a chromatographic surface including a hydrophobic surface group and one or more ionizable modifiers, and a second solvent comprising an acid; and (iv) analyzing the component of the first fraction by mass spectroscopy, thereby identifying the polypeptide, if present, using a signal corresponding to a sequence fragment ion from the polypeptide. The signal can correspond to an intact multiply charged precursor fragment selected in a first quadrupole and its corresponding sequence fragment ion selected in a final quadrupole.

Abstract translation: 用于鉴定样品多肽的方法可以包括（i）用疑似含有胰岛素的试样与碱处理; （ii）使用混合模式或聚合反相介质和包含酸的第一溶剂通过固相萃取提取处理过的样品的第一级分; （iii）使用包括疏水性表面基团和一种或多种可离子化改性剂的色谱表面的液相色谱法和包含酸的第二溶剂分离第一级分的组分; 和（iv）通过质谱法分析第一级分的组分，从而使用对应于来自多肽的序列片段离子的信号鉴定多肽（如果存在）。 该信号可以对应于在第一个四极中选择的完整的多电荷前体片段及其在最终四极中选择的相应的序列片段离子。