目的建立全血中除草剂百草枯的高效液相色谱-四级杆串联飞行时间质谱（LC-Q/TOF）的检验方法。方法用乙腈提取样品中的百草枯,以乙腈（0.1%甲酸）-50mmol·L-1醋酸铵水溶液（甲酸调p H 3.5）为流动相,梯度洗脱,经RX-SIL色谱柱（2.1&...目的建立全血中除草剂百草枯的高效液相色谱-四级杆串联飞行时间质谱（LC-Q/TOF）的检验方法。方法用乙腈提取样品中的百草枯,以乙腈（0.1%甲酸）-50mmol·L-1醋酸铵水溶液（甲酸调p H 3.5）为流动相,梯度洗脱,经RX-SIL色谱柱（2.1×100mm,1.8μm）分离,以电喷雾离子源正离子模式采集全扫描及MS/MS数据进行分析。结果该方法灵敏度达5.0μg·L-1,在10.0-1000.0μg·L-1范围内线性关系良好;低、中、高3种浓度的加样回收率分别为90.5%、91.5%、87.4%,相对标准偏差（RSD）均小于10%。结论该法操作简单、灵敏度高,结果可靠,完全满足公安机关在办理百草枯中毒案件中的需要。展开更多
Forced degradation study of argatroban under conditions of hydrolysis(neutral, acidic and alkaline), oxidation,photolysis and thermal stress, as suggested in the ICH Q1 A(R2), was accomplished. The drug showed signifi...Forced degradation study of argatroban under conditions of hydrolysis(neutral, acidic and alkaline), oxidation,photolysis and thermal stress, as suggested in the ICH Q1 A(R2), was accomplished. The drug showed significant degradation under hydrolysis(acidic, alkaline) and oxidation(peroxide stress) conditions. The drug remained stable under thermal and photolytic stress conditions. In total, seven novel degradation products(DP-1 to DP-7) were found under diverse conditions, which were not reported earlier. The chemical structures of these degradation products were characterized by ~1H NMR,^(13)C NMR, 2 D NMR, Q-TOF-MSnand IR spectral analysis and the proposed degradation products structures were further confirmed by the individual synthesis.展开更多
文摘目的建立全血中除草剂百草枯的高效液相色谱-四级杆串联飞行时间质谱（LC-Q/TOF）的检验方法。方法用乙腈提取样品中的百草枯,以乙腈（0.1%甲酸）-50mmol·L-1醋酸铵水溶液（甲酸调p H 3.5）为流动相,梯度洗脱,经RX-SIL色谱柱（2.1×100mm,1.8μm）分离,以电喷雾离子源正离子模式采集全扫描及MS/MS数据进行分析。结果该方法灵敏度达5.0μg·L-1,在10.0-1000.0μg·L-1范围内线性关系良好;低、中、高3种浓度的加样回收率分别为90.5%、91.5%、87.4%,相对标准偏差（RSD）均小于10%。结论该法操作简单、灵敏度高,结果可靠,完全满足公安机关在办理百草枯中毒案件中的需要。
文摘Forced degradation study of argatroban under conditions of hydrolysis(neutral, acidic and alkaline), oxidation,photolysis and thermal stress, as suggested in the ICH Q1 A(R2), was accomplished. The drug showed significant degradation under hydrolysis(acidic, alkaline) and oxidation(peroxide stress) conditions. The drug remained stable under thermal and photolytic stress conditions. In total, seven novel degradation products(DP-1 to DP-7) were found under diverse conditions, which were not reported earlier. The chemical structures of these degradation products were characterized by ~1H NMR,^(13)C NMR, 2 D NMR, Q-TOF-MSnand IR spectral analysis and the proposed degradation products structures were further confirmed by the individual synthesis.
