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建立了液相色谱-四极杆-飞行时间质谱法(LC-Q-TOF-MS)结合氯铬酸吡啶(PCC)氧化反应对熊胆粉中2个新同分异构体进行结构确证。取熊去氧胆酸(UDCA)对照品和鹅去氧胆酸(CDCA)对照品,经PCC氧化后,用LC-Q-TOF-MS分析氧化物。再取熊胆粉样品,以甲醇提取后供LC-Q-TOF-MS测定。采用Agilent Zorbax SB C18色谱柱(2.1 mm×100 mm,1.8μm),流动相为乙腈-0.1%甲酸溶液(45∶55)。质谱采用正离子、负离子、MS及MS/MS模式分别测定。根据PCC可将仲醇氧化成酮的特性、UDCA与CDCA的立体异构性,可确证各氧化物的化学结构,并以确证结果对熊胆粉中2个新同分异构体进行鉴别,结果鉴别出熊胆粉中含3α-羟基-7-氧代-5β-胆烷酸和7α-羟基-3-氧代-5β-胆烷酸2个新胆汁酸。
A new LC-Q-TOF-MS coupled with PCC oxidation was developed for the structural elucidation of two new isomers in bovine gall powder. The ursodeoxycholic acid (UDCA) reference and chenodeoxycholic acid (CDCA) control were taken and oxidized with PCC, followed by analysis of the oxide by LC-Q-TOF-MS. Bear gall powder samples were taken and extracted with methanol for LC-Q-TOF-MS determination. Agilent Zorbax SB C18 column (2.1 mm × 100 mm, 1.8 μm) was used with a mobile phase of acetonitrile-0.1% formic acid (45:55). The mass spectra were determined by positive ion, negative ion, MS and MS / MS respectively. According to PCC secondary alcohol can be oxidized to ketones characteristics, UDCA and CDCA stereoisomerism, confirm the chemical structure of each oxide, and confirm the results of two new isomers of bear bile powder identification, As a result, two new bile acids containing 3α-hydroxy-7-oxo-5β-cholanoic acid and 7α-hydroxy-3-oxo-5β-cholanoic acid were identified.