【摘要】 环磷酸腺苷(cAMP)是大枣中特色最为突出的重要生物活性物质,本研究建立了超声辅助提取-亲水色谱-二极管阵列检测器-电喷雾四极杆飞行时间质谱法(UAE-HILIC-DAD-ESI-Q-TOF/MS)定性定量测定大枣中cAMP的方法。采用超声辅助提取法用于cAMP的提取,采用Waters Xbridge Amide(250 mm×4.6 mm,3.5μm)亲水色谱柱进行分离,以乙腈和20 mmol/L CH3COONH4+0.2%CH3COOH为流动相,流速0.8 mL/min,柱温为室温。采用电喷雾四极杆飞行时间质谱,在正离子模式下,进行分析。采用超声提取法,cAMP的提取率较高;在优化的亲水色谱条件下,大枣水提物中cAMP与其他化合物分离良好;根据电喷雾四极杆飞行时间质谱获得的母离子和子离子的精确分子量信息,结合标准对照品的保留时间和UV信息可以对其进行准确鉴别。cAMP在0.01μg/mL～50.00μg/mL范围内具有良好的线性关系(r2=0.999 1),采用发展的方法用于金丝小枣与大红枣中的cAMP的含量测定。本文发展的UVE-HILIC-DAD-ESI-Q-TOF/MS测定大枣中cAMP的方法,分离度好、灵敏度高,为快速鉴别和测定大枣中的cAMP及资源开发研究提供了分析测定方法支持。更多还原

【Abstract】 A new method has been developed based on ultrasound-assisted extraction(UAE) followed by hydrophilic interaction chromatography(HILIC) and electrospray ionization-quadrupole-time of flight mass spectrometry(ESI-Q-TOF/MS) for the determination of cAMP in the extracts of fructus jujubae.The separation was achieved on a Waters Xbridge Amide column(250 × 4.6 mm I.D.,3.5 μm) andgradient elution using a solution of acetonitrile and 20 mmol/L CH3COONH4 +0.2% CH3 COOH as the mobile phase.Identification of the cAMP was based on retention time,UV spectra,and mass measurements of the protonated molecules([M+H]+) and main fragment ions(ESI-Q-TOF/MS).The cAMP was quantified by HILIC-DAD under optimized chromatography conditions.The linear ranger for cAMP was 0.01 μg/mL-50.00 μg/mL,and the calibration curve showedgood linearity(r2= 0.999 1).The developed method was applied to quantify the target compound in Golden silk Jujube and Jujube.The developed HILIC-DAD-ESI-Q-TOF/MS method has potential applicability for the identification and determination of highly polar active compounds and quality control of fructus jujubae.更多还原