目的将实时直接分析离子源(direct analysis in real time,DART)与三重四极杆质谱联用,建立食品中非法添加PDE-5型抑制剂的快速筛查方法。方法3种不同基质样品加入乙腈振摇10 s后,设进样速率0.2 mm/s,进样体积4μl,选择DART离子源,离子...目的将实时直接分析离子源(direct analysis in real time,DART)与三重四极杆质谱联用,建立食品中非法添加PDE-5型抑制剂的快速筛查方法。方法3种不同基质样品加入乙腈振摇10 s后,设进样速率0.2 mm/s,进样体积4μl,选择DART离子源,离子化温度450℃,在正离子、多反应监测(MRM)下进行检测。结果该方法7种物质的检出限为0.025~12.5μg/g,检出阳性样品4种,分别非法添加羟基卡巴地那非、环己基去甲他达拉非、N-苄基他达拉非和N-苯基丙氧苯基卡巴地那非。结论该方法样品前处理简单,分析速度快,定性准确,环境污染小,能满足食品中非法添加PDE-5型抑制剂的快速筛查要求。展开更多
建立了高效液相色谱串联质谱仪对酒类产品中11种PDE-5抑制剂及其衍生剂的快速分析方法。样品经乙腈∶水(1∶1,v/v)超声提取,Atlantis d C_(18)色谱柱(2.1×150 mm,3μm)为分析柱,0.1%甲酸溶液和0.1%甲酸乙腈为流动相,电喷雾正离子...建立了高效液相色谱串联质谱仪对酒类产品中11种PDE-5抑制剂及其衍生剂的快速分析方法。样品经乙腈∶水(1∶1,v/v)超声提取,Atlantis d C_(18)色谱柱(2.1×150 mm,3μm)为分析柱,0.1%甲酸溶液和0.1%甲酸乙腈为流动相,电喷雾正离子多反应监测模式进行检测,外标法定量。试验结果表明,该方法的RSD值范围为0.57%~11.69%,回收率范围在60.0%~118.6%,该方法的线性相关性良好,检测低限、精密度和准确度均符合要求,能够满足酒类产品中11种PDE-5抑制剂及其衍生剂的检测要求。展开更多
Counterfeit medicines are a growing problem in both developing and industrialised countries. In general the evaluation of these medicines is limited to the identification and the dosage of the active ingredients. In t...Counterfeit medicines are a growing problem in both developing and industrialised countries. In general the evaluation of these medicines is limited to the identification and the dosage of the active ingredients. In this study in vitro dissolution tests were conducted on two sets of counterfeit medicines containing PDE-5 inhibitors （sildenafil citrate and tadalafil）. The dissolution profiles were statistically compared to the ones of the genuine products using the f2-method and a comparison at each time point using the Cochran test. The results showed low equivalences between counterfeit and genuine products as well as higher variations around the mean dissolution value at the different time points for the counterfeit products.展开更多
文摘目的将实时直接分析离子源(direct analysis in real time,DART)与三重四极杆质谱联用,建立食品中非法添加PDE-5型抑制剂的快速筛查方法。方法3种不同基质样品加入乙腈振摇10 s后,设进样速率0.2 mm/s,进样体积4μl,选择DART离子源,离子化温度450℃,在正离子、多反应监测(MRM)下进行检测。结果该方法7种物质的检出限为0.025~12.5μg/g,检出阳性样品4种,分别非法添加羟基卡巴地那非、环己基去甲他达拉非、N-苄基他达拉非和N-苯基丙氧苯基卡巴地那非。结论该方法样品前处理简单,分析速度快,定性准确,环境污染小,能满足食品中非法添加PDE-5型抑制剂的快速筛查要求。
文摘建立了高效液相色谱串联质谱仪对酒类产品中11种PDE-5抑制剂及其衍生剂的快速分析方法。样品经乙腈∶水(1∶1,v/v)超声提取,Atlantis d C_(18)色谱柱(2.1×150 mm,3μm)为分析柱,0.1%甲酸溶液和0.1%甲酸乙腈为流动相,电喷雾正离子多反应监测模式进行检测,外标法定量。试验结果表明,该方法的RSD值范围为0.57%~11.69%,回收率范围在60.0%~118.6%,该方法的线性相关性良好,检测低限、精密度和准确度均符合要求,能够满足酒类产品中11种PDE-5抑制剂及其衍生剂的检测要求。
文摘Counterfeit medicines are a growing problem in both developing and industrialised countries. In general the evaluation of these medicines is limited to the identification and the dosage of the active ingredients. In this study in vitro dissolution tests were conducted on two sets of counterfeit medicines containing PDE-5 inhibitors （sildenafil citrate and tadalafil）. The dissolution profiles were statistically compared to the ones of the genuine products using the f2-method and a comparison at each time point using the Cochran test. The results showed low equivalences between counterfeit and genuine products as well as higher variations around the mean dissolution value at the different time points for the counterfeit products.
