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
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.
文摘建立了高效液相色谱-电喷雾串联质谱(HPLC-ESI MS/MS)分析环境水样中22种抗生素类药物的方法。采用HLB固相萃取柱对环境水样中的目标化合物进行富集、净化,然后以6mL氨水-甲醇(5∶95,v/v)溶液洗脱。收集的洗脱液经氮气吹干至1mL,然后进行HPLC-ESI MS/MS分离分析。色谱流动相A相为甲醇-乙腈(1∶1,v/v),B相为0.3%(体积分数)甲酸水溶液(含0.1%(体积分数)甲酸铵,pH2.9);色谱柱为XTerra MS C18柱。质谱检测采用正离子扫描,多反应监测模式。分别以自来水和污水作为基质,22种抗生素类药物的加标平均回收率分别为54.9%～130%和57.4%～138%,相对标准偏差(n=3)分别为2.85%～28.6%和2.02%～23.2%;方法的检出限为0.05～0.5ng/L。将建立的方法应用于北京市高碑店湖和小清河水样的分析,结果表明在两个水样中均有部分抗生素类药物检出。
