广州化工
廣州化工
엄주화공
GUANGZHOU CHEMICAL INDUSTRY AND TECHNOLOGY
2014年
19期
105-107
,共3页
阿齐沙坦%降解产物%高效液相色谱-串联质谱
阿齊沙坦%降解產物%高效液相色譜-串聯質譜
아제사탄%강해산물%고효액상색보-천련질보
azilsartan%degradation compounds%LC-MS
以1%甲酸溶液-乙腈为流动相,经C18柱(250 mm ×4.6 mm,5μm)分离,通过串联ESI质谱在线检测,获得相关的色谱和质谱信息。根据研究结果推测光降解主要产物为1-((2′-1H-双吖丙啶-3-基-[1,1′-联苯]-4-基)甲基)-2-乙氧基-1H-苯并[d]咪唑-7-羧酸,酸降解主要产物为2-氧代-3-((2′-(5-氧代-4,5-二氢-1,2,4-噁二唑酮-3-基)-[1,1′-联苯]-4-基)甲基)-2,3-二氢-1H-苯并[d]咪唑-4-羧酸。
以1%甲痠溶液-乙腈為流動相,經C18柱(250 mm ×4.6 mm,5μm)分離,通過串聯ESI質譜在線檢測,穫得相關的色譜和質譜信息。根據研究結果推測光降解主要產物為1-((2′-1H-雙吖丙啶-3-基-[1,1′-聯苯]-4-基)甲基)-2-乙氧基-1H-苯併[d]咪唑-7-羧痠,痠降解主要產物為2-氧代-3-((2′-(5-氧代-4,5-二氫-1,2,4-噁二唑酮-3-基)-[1,1′-聯苯]-4-基)甲基)-2,3-二氫-1H-苯併[d]咪唑-4-羧痠。
이1%갑산용액-을정위류동상,경C18주(250 mm ×4.6 mm,5μm)분리,통과천련ESI질보재선검측,획득상관적색보화질보신식。근거연구결과추측광강해주요산물위1-((2′-1H-쌍아병정-3-기-[1,1′-련분]-4-기)갑기)-2-을양기-1H-분병[d]미서-7-최산,산강해주요산물위2-양대-3-((2′-(5-양대-4,5-이경-1,2,4-오이서동-3-기)-[1,1′-련분]-4-기)갑기)-2,3-이경-1H-분병[d]미서-4-최산。
The HPLC separation experiments were performed on aC 18 column (250mm ×4.6mm, 5μm), with 1%formic acid-acetonitrile as mobile phase.The analytics were determined by ESI -MS.The chromatograms and mass spectra of forced degradation products of azilsartan were obtained by LC -MS.The structure of impurities were confirmed as 1-((2'-(1H-diazirin-3-yl) -[1,1'-biphenyl] -4-yl)methyl) -2-ethoxy-1H-benzo[d] imidazole-7-carboxylic acid, 2-oxo-3-((2'-(5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl) -[1,1'-biphenyl] -4-yl)methyl)-2,3-dihydro-1H-benzo[d] imidazole-4-carboxylic acid, respectively.