中国中药杂志

2013, v.38(14) 2338-2342

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LC-Q-TOF-MS结合PCC氧化反应快速鉴别熊胆粉中的2个新同分异构体
Rapid identification of two new isomers in bear bile powder by LC-Q-TOF-MS combined with PCC oxidation

简龙海;胡青;于泓;王柯;季申;
JIAN Long-hai,HU Qing,YU Hong,WANG Ke,JI Shen(Shanghai Institute for Food and Drug Control,Shanghai 201203,China)

摘要(Abstract):

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 rapid method of Liquid chromatography-quadrupole time-of-flight mass spectrometry(LC-Q-TOF-MS) combined with pyridinium chlorochromate(PCC) oxidation has been developed to determine chemical structures of two novel isomers in bear bile powder.Derivatives of ursodeoxycholic acid(UDCA) and chenodeoxycholic acid(CDCA) were semi-synthesized by PCC oxidation,then were analyzed by LC-Q-TOF-MS.Separation was carried out on a reverse column with the mobile phase of acetonitrile-0.1% formic acid(45∶55).The data of Q-TOF-MS was acquired by MS,MS/MS,positive and negative modes.Since UDCA and CDCA were stereochemical isomeric at an alcohol position,two oxidation products were same and have been confirmed by LC-Q-TOF-MS.Other two products were also determined based on the PCC oxidation theory.Samples of bear bile powder were dissolved by methanol and measured by LC-Q-TOF-MS.Two unknown peaks were found and identified by matching their retention times and accurate mass spectra ions with PCC oxidation productS.Finally,the structures of two new bile acids in bear bile powder were confirmed as 3α-hydroxy-7-oxo-5β-cholanic acid,7α-hydroxy-3-oxo-5β-cholanic acid,respectively.

关键词(KeyWords): 熊胆粉;熊去氧胆酸;鹅去氧胆酸;氯铬酸吡啶;液相色谱-四极杆-飞行时间质谱;鉴别
bear bile powder;ursodeoxycholic acid;chenodeoxycholic acid;pyridinium chlorochromate;LC-Q-TOF;identification

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作者(Author): 简龙海;胡青;于泓;王柯;季申;
JIAN Long-hai,HU Qing,YU Hong,WANG Ke,JI Shen(Shanghai Institute for Food and Drug Control,Shanghai 201203,China)

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