建立了高效液相色谱-电喷雾-四级杆飞行时间质谱(HPLC-ESI-Q-TOF)分析高粱多酚的方法。色谱条件为:流动相A为体积分数为0.1%甲酸的H_(2)O,流动相B为体积分数为0.1%甲酸的乙腈,流动相梯度A 0~20 min 85%~40%、20~23 min 40%~10%、23~28 m...建立了高效液相色谱-电喷雾-四级杆飞行时间质谱(HPLC-ESI-Q-TOF)分析高粱多酚的方法。色谱条件为:流动相A为体积分数为0.1%甲酸的H_(2)O,流动相B为体积分数为0.1%甲酸的乙腈,流动相梯度A 0~20 min 85%~40%、20~23 min 40%~10%、23~28 min 10%~10%、28~30 min 10%~85%、30~37 min 85%~85%;流速0.2 mL/min,进样量5μL,柱温30℃。质谱条件为:负离子模式下,毛细管电压2.6 kV,干燥气温度180℃,干燥气流量6 L/min,辅助气压力0.08 MPa,质荷比采集范围100~1200 m/z,碰撞能量为35 eV。对5种高粱所含的多酚类物质进行分析,共鉴定出20种高粱多酚,包括10种酚酸类物质、3种原花青素、7种酚酸类衍生物。展开更多
In this paper, we proposed a novel resolution criterion(improved calibrated normalized resolution product, r*') to evaluate separation quality of fingerprints. By comparing with the calibrated normalized resolutio...In this paper, we proposed a novel resolution criterion(improved calibrated normalized resolution product, r*') to evaluate separation quality of fingerprints. By comparing with the calibrated normalized resolution product(r*) and the hierarchical chromatographic response function(HCRF), the validity of this criterion was demonstrated by experimental chromatograms. The soy isoflavone extract was selected as the analytical object. The initial and end percentages of methanol and elution time affecting gradient elution were tested by orthogonal design. The final optimized conditions were as follows. It was detected by UV absorbance at 254 nm, column temperature was maintained at 36 oC, solvent A was 0.1%(v/v) acetic acid, solvent B was methanol, gradient elution was from 34% to 65% B in a linear gradient in 25 min, and the flow-rate was set at 1.0 m L/min. In addition, the main ingredients of the soy isoflavone extract were confirmed by LC-ESI/MS.展开更多
文摘建立了高效液相色谱-电喷雾-四级杆飞行时间质谱(HPLC-ESI-Q-TOF)分析高粱多酚的方法。色谱条件为:流动相A为体积分数为0.1%甲酸的H_(2)O,流动相B为体积分数为0.1%甲酸的乙腈,流动相梯度A 0~20 min 85%~40%、20~23 min 40%~10%、23~28 min 10%~10%、28~30 min 10%~85%、30~37 min 85%~85%;流速0.2 mL/min,进样量5μL,柱温30℃。质谱条件为:负离子模式下,毛细管电压2.6 kV,干燥气温度180℃,干燥气流量6 L/min,辅助气压力0.08 MPa,质荷比采集范围100~1200 m/z,碰撞能量为35 eV。对5种高粱所含的多酚类物质进行分析,共鉴定出20种高粱多酚,包括10种酚酸类物质、3种原花青素、7种酚酸类衍生物。
基金National Higher-Education Institution General Research and Development Funding(Grant No.JKP2011010)
文摘In this paper, we proposed a novel resolution criterion(improved calibrated normalized resolution product, r*') to evaluate separation quality of fingerprints. By comparing with the calibrated normalized resolution product(r*) and the hierarchical chromatographic response function(HCRF), the validity of this criterion was demonstrated by experimental chromatograms. The soy isoflavone extract was selected as the analytical object. The initial and end percentages of methanol and elution time affecting gradient elution were tested by orthogonal design. The final optimized conditions were as follows. It was detected by UV absorbance at 254 nm, column temperature was maintained at 36 oC, solvent A was 0.1%(v/v) acetic acid, solvent B was methanol, gradient elution was from 34% to 65% B in a linear gradient in 25 min, and the flow-rate was set at 1.0 m L/min. In addition, the main ingredients of the soy isoflavone extract were confirmed by LC-ESI/MS.