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高效液相色谱/串联质谱法鉴定水溶液制剂中的鲑鱼降钙素降解产物

High-performance liquid chromatography/tandem mass spectrometry identification of salmon calcitonin degradation products in aqueous solution preparations.

作者信息

Silvestro L, Savu S R

机构信息

Res Pharma Pharmacological Research S.r.1, Torino, Italy.

出版信息

Rapid Commun Mass Spectrom. 1996;10(2):151-6. doi: 10.1002/(SICI)1097-0231(19960131)10:2<151::AID-RCM434>3.0.CO;2-C.

DOI:10.1002/(SICI)1097-0231(19960131)10:2<151::AID-RCM434>3.0.CO;2-C
PMID:8616264
Abstract

Degradation impurities have been investigated, by means of high-performance liquid chromatography (HPLC)/ mass spectrometry, in commercial ampoules of salmon calcitonin, aqueous solution, stored for up to 2 years. Oxidation derivatives of the cysteine residues in positions 1 and 7, with cleavage of the disulfide bridge, were observed in all samples. Using our reversed-phase separation, these oxidation derivatives coeluted and presented an HPLC behavior identical to the derivative of salmon calcitonin with the disulfide bridge reduced. In a previous study this last compound was tentatively identified, without confirmation by mass spectrometry, as a major degradation product of salmon calcitonin in aqueous solution.

摘要

通过高效液相色谱(HPLC)/质谱法,对储存长达2年的市售鲑鱼降钙素水溶液安瓿中的降解杂质进行了研究。在所有样品中均观察到1位和7位半胱氨酸残基的氧化衍生物,二硫键断裂。使用我们的反相分离方法,这些氧化衍生物共洗脱,并且呈现出与二硫键还原的鲑鱼降钙素衍生物相同的HPLC行为。在先前的一项研究中,未经质谱确认,该最后一种化合物被初步鉴定为鲑鱼降钙素在水溶液中的主要降解产物。

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