A rapid method based on rapid resolution liquid chromatography（RRLC） coupled with a diode array detector（DAD） was developed for the simultaneous determination of six major constituents（magnoflorine,jatrorrhizine,...A rapid method based on rapid resolution liquid chromatography（RRLC） coupled with a diode array detector（DAD） was developed for the simultaneous determination of six major constituents（magnoflorine,jatrorrhizine,coptisine,palmatine,berberine and evodiamine） in traditional Chinese medicine（TCM） Zuo Jin Pill（ZJP）.The satisfactory chromatographic separation was carried on an Eclipse Plus C18 column（1.8 μm i.d.,150 mm×4.6 mm） by linear gradient elution with a mobile phase of acetonitrile-acetate buffer.All the calibration curves show good linearity（r2 0.9998）.The detection limits and quantification limits ranged in 1.4―12 ng and 4.8―30 ng,respectively.The intra-and inter-day precisions were less than 0.63% with accuracies 98.60%―100.78%,and the recoveries were from 99.45% to 100.46%.Furthermore,hierarchical cluster analysis（HCA） was used to evaluate the variation of the herbal prescription.The results demonstrate that this analytical method is simple,sensitive and reliable for rapidly analyzing six major bioactive compounds in ZJPs and is helpful to comprehensively evaluating the quality of this TCM.展开更多
Background Stomach cancer is among the most commonly occurring malignancies worldwide. It would be beneficial to develop a urine-based assay whereby patients with undiagnosed stomach cancer could be screened and their...Background Stomach cancer is among the most commonly occurring malignancies worldwide. It would be beneficial to develop a urine-based assay whereby patients with undiagnosed stomach cancer could be screened and their cancer detected in the eadiest stages. Methods A urinary metabonomics method based on ultra-performance liquid chromatography combined with quadruple time-of-flight mass spectrometry was used to analyze urine samples from patients with stomach cancer and healthy controls. Results Statistical analysis revealed a clear separation of patients and healthy controls using the aforementioned methodology. Some significantly changed metabolites were identified. Conclusions Use of the metabonomics method in patients with stomach cancer could effectively detect distinct changes in urinary metabolites and had the capacity to detect cancer; therefore, it may be a valuable tool in earlier diagnosis. Furthermore, the detection and identification of altered metabolites in the current study may help elucidate possible mechanisms involved in stomach cancer.展开更多
目的:建立快速高分辩液相色谱(RRLC)同时测定天王补心丸中五味子醇甲、五味子醇乙、五味子酯甲、五味子甲素、五味子乙素、五味子丙素6种主要木脂素成分的方法。方法:采用TSK gel ODS-140HTP(50 mm×2.1 mm,2.3μm)色谱柱;流动相为...目的:建立快速高分辩液相色谱(RRLC)同时测定天王补心丸中五味子醇甲、五味子醇乙、五味子酯甲、五味子甲素、五味子乙素、五味子丙素6种主要木脂素成分的方法。方法:采用TSK gel ODS-140HTP(50 mm×2.1 mm,2.3μm)色谱柱;流动相为乙腈-水梯度洗脱,流速0.3 m L·min-1;柱温30℃;检测波长250 nm,进样量10μL。结果:6种被测木脂素成分分离度良好;各成分质量与峰面积在测定范围内均呈良好的线性关系(r>0.9990),重复性良好;平均回收率分别为100.1%、99.3%、97.8%、99.1%、98.8%、97.5%,RSD分别为1.1%、1.8%、2.3%、2.5%、1.6%、2.1%。结论:此方法简便、准确、重复性好,经方法学验证可用于检测天王补心丸的质量。展开更多
基金Supported by the National Natural Science Foundation of China(No.30725045)the Special Program for New Drug Innovation of the Ministry of Science and Technology,China(Nos.2009ZX09311-001 and 2008ZX09101-Z-029)+2 种基金China Postdoctoral Science Foundation(No.20080441304)Shanghai Leading Academic Discipline Project,China(No.B906)the Scientific Foundation of Shanghai City,China(Nos.07DZ19728,09DZ1975700 and 09DZ1971500)
文摘A rapid method based on rapid resolution liquid chromatography（RRLC） coupled with a diode array detector（DAD） was developed for the simultaneous determination of six major constituents（magnoflorine,jatrorrhizine,coptisine,palmatine,berberine and evodiamine） in traditional Chinese medicine（TCM） Zuo Jin Pill（ZJP）.The satisfactory chromatographic separation was carried on an Eclipse Plus C18 column（1.8 μm i.d.,150 mm×4.6 mm） by linear gradient elution with a mobile phase of acetonitrile-acetate buffer.All the calibration curves show good linearity（r2 0.9998）.The detection limits and quantification limits ranged in 1.4―12 ng and 4.8―30 ng,respectively.The intra-and inter-day precisions were less than 0.63% with accuracies 98.60%―100.78%,and the recoveries were from 99.45% to 100.46%.Furthermore,hierarchical cluster analysis（HCA） was used to evaluate the variation of the herbal prescription.The results demonstrate that this analytical method is simple,sensitive and reliable for rapidly analyzing six major bioactive compounds in ZJPs and is helpful to comprehensively evaluating the quality of this TCM.
文摘Background Stomach cancer is among the most commonly occurring malignancies worldwide. It would be beneficial to develop a urine-based assay whereby patients with undiagnosed stomach cancer could be screened and their cancer detected in the eadiest stages. Methods A urinary metabonomics method based on ultra-performance liquid chromatography combined with quadruple time-of-flight mass spectrometry was used to analyze urine samples from patients with stomach cancer and healthy controls. Results Statistical analysis revealed a clear separation of patients and healthy controls using the aforementioned methodology. Some significantly changed metabolites were identified. Conclusions Use of the metabonomics method in patients with stomach cancer could effectively detect distinct changes in urinary metabolites and had the capacity to detect cancer; therefore, it may be a valuable tool in earlier diagnosis. Furthermore, the detection and identification of altered metabolites in the current study may help elucidate possible mechanisms involved in stomach cancer.
文摘目的:建立快速高分辩液相色谱(RRLC)同时测定天王补心丸中五味子醇甲、五味子醇乙、五味子酯甲、五味子甲素、五味子乙素、五味子丙素6种主要木脂素成分的方法。方法:采用TSK gel ODS-140HTP(50 mm×2.1 mm,2.3μm)色谱柱;流动相为乙腈-水梯度洗脱,流速0.3 m L·min-1;柱温30℃;检测波长250 nm,进样量10μL。结果:6种被测木脂素成分分离度良好;各成分质量与峰面积在测定范围内均呈良好的线性关系(r>0.9990),重复性良好;平均回收率分别为100.1%、99.3%、97.8%、99.1%、98.8%、97.5%,RSD分别为1.1%、1.8%、2.3%、2.5%、1.6%、2.1%。结论:此方法简便、准确、重复性好,经方法学验证可用于检测天王补心丸的质量。
