目的应用UHPLC/QTOF-MS对紫金锭提取物中的化学成分进行鉴定。方法色谱分离采用Agilent Eclipse Plus C18色谱柱(100mm×2.1mm,3.5μm),0.1%甲酸水溶液-乙腈梯度洗脱。质谱分析采用电喷雾离子源,负离子模式检测。结果通过二级质谱...目的应用UHPLC/QTOF-MS对紫金锭提取物中的化学成分进行鉴定。方法色谱分离采用Agilent Eclipse Plus C18色谱柱(100mm×2.1mm,3.5μm),0.1%甲酸水溶液-乙腈梯度洗脱。质谱分析采用电喷雾离子源,负离子模式检测。结果通过二级质谱裂解分析以及文献信息比对,从紫金锭中鉴定出了没食子酸、间二没食子酸、没食子酸甲酯、七叶内酯、柚皮苷、1,2,3,4,6-O-五没食子酰葡萄糖、1,4-二4-(葡萄糖氧)苄基-2-异丁基苹果酸酯、淫羊藿糖甙、Sarcogenin,大豆苷元、乌索酸等11个化合物。结论本法为紫金锭的化学成分鉴定提供快速和准确方法。展开更多
目的建立一种基于固相萃取-高效液相色谱串联四级杆飞行时间质谱检测人全血中马钱子碱的检测方法。方法样品过Oasis HLB固相萃取小柱,经3 m L去离子水淋洗,有机溶剂洗脱后,在Zorbox Eclipse Plus C18（2.1mm×50mm,1.8μm）色谱柱...目的建立一种基于固相萃取-高效液相色谱串联四级杆飞行时间质谱检测人全血中马钱子碱的检测方法。方法样品过Oasis HLB固相萃取小柱,经3 m L去离子水淋洗,有机溶剂洗脱后,在Zorbox Eclipse Plus C18（2.1mm×50mm,1.8μm）色谱柱上分离,以0.1%甲酸水溶液-甲醇为流动相梯度洗脱,流速为0.3 m L/min,四级杆飞行时间串联质谱检测。通过计算500 ng/m L马钱子碱对照样品在上述固相萃取和色谱质谱条件下,不同洗脱溶剂以及不同洗脱体积下的回收效率从而优化洗脱溶剂的种类和使用量。结果以甲醇为洗脱溶剂,加入量为3 m L时,马钱子碱在200-2000 ng/m L的添加水平下回收率为80.1%-101.3%,相对标准偏差为5.2%-8.3%。人全血中马钱子碱在50-5000 ng/m L范围内线性良好（R^2=0.999 97）,检测限为10.2 ng/m L,最低定量限为34.1 ng/m L。结论该方法快速方便,回收率和灵敏度高,可用于人全血中马钱子碱的定量测定。展开更多
Phyllanthus species plants are a rich source of phenolics and widely used due to their medicinal properties. A liquid chromatography–tandem mass spectrometry(LC–MS/MS) method was developed using high-pressure liquid...Phyllanthus species plants are a rich source of phenolics and widely used due to their medicinal properties. A liquid chromatography–tandem mass spectrometry(LC–MS/MS) method was developed using high-pressure liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry(HPLC-ESI-QTOFMS/MS) for the identification and characterization of quercetin, kaempferol, ellagic acid and their derivatives in ethanolic extracts of Phyllanthus species. The chromatographic separation was carried out on Thermo Betasil C_8 column(250 mm×4.5 mm, 5 μm) using 0.1% formic acid in water and 0.1% formic acid in methanol as the mobile phase. The identification of diagnostic fragment ions and optimization of collision energies were carried out using 21 reference standards. Totally 51 compounds were identified which include 21 compounds identified and characterized unambiguously by comparison with their authentic standards and the remaining 30 were tentatively identified and characterized in ethanolic extracts of P. emblica, P. fraternus, P. amarus and P.niruri.展开更多
文摘目的应用UHPLC/QTOF-MS对紫金锭提取物中的化学成分进行鉴定。方法色谱分离采用Agilent Eclipse Plus C18色谱柱(100mm×2.1mm,3.5μm),0.1%甲酸水溶液-乙腈梯度洗脱。质谱分析采用电喷雾离子源,负离子模式检测。结果通过二级质谱裂解分析以及文献信息比对,从紫金锭中鉴定出了没食子酸、间二没食子酸、没食子酸甲酯、七叶内酯、柚皮苷、1,2,3,4,6-O-五没食子酰葡萄糖、1,4-二4-(葡萄糖氧)苄基-2-异丁基苹果酸酯、淫羊藿糖甙、Sarcogenin,大豆苷元、乌索酸等11个化合物。结论本法为紫金锭的化学成分鉴定提供快速和准确方法。
基金CSIR, New Delhi, India, for financial supportBK for NMPB grant GO/UP/03/09
文摘Phyllanthus species plants are a rich source of phenolics and widely used due to their medicinal properties. A liquid chromatography–tandem mass spectrometry(LC–MS/MS) method was developed using high-pressure liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry(HPLC-ESI-QTOFMS/MS) for the identification and characterization of quercetin, kaempferol, ellagic acid and their derivatives in ethanolic extracts of Phyllanthus species. The chromatographic separation was carried out on Thermo Betasil C_8 column(250 mm×4.5 mm, 5 μm) using 0.1% formic acid in water and 0.1% formic acid in methanol as the mobile phase. The identification of diagnostic fragment ions and optimization of collision energies were carried out using 21 reference standards. Totally 51 compounds were identified which include 21 compounds identified and characterized unambiguously by comparison with their authentic standards and the remaining 30 were tentatively identified and characterized in ethanolic extracts of P. emblica, P. fraternus, P. amarus and P.niruri.
