液相31P核磁共振(phosphorus-31 nuclear magnetic resonance,31P-NMR)是近年来用于分析沉积物有机磷组成的新技术.本研究围绕31P-NMR分析沉积物样品的制备过程(包括样品前处理方法、提取时间、提取剂比例、样品浓缩等)进行探讨.结果表...液相31P核磁共振(phosphorus-31 nuclear magnetic resonance,31P-NMR)是近年来用于分析沉积物有机磷组成的新技术.本研究围绕31P-NMR分析沉积物样品的制备过程(包括样品前处理方法、提取时间、提取剂比例、样品浓缩等)进行探讨.结果表明,采用风干的沉积物样品进行提取,磷的提取效率明显提高.提取过程中,沉积物磷的释放主要在前8 h,为提高磷的提取效率,可将提取时间延长至12～16 h.提取比例[m(沉积物)∶V(提取剂)]1∶8与1∶20相比,在浓缩倍数相同的情况下,前者获得的31P-NMR信号峰多于后者,因此提取比例倾向于使用1∶8.提取液样品在28℃下旋转蒸发浓缩,并经低温离心后,磷无显著损失.展开更多
目的采用加氧附件-有机进样系统建立了 IC P - M S 直接进样测定食用油中铅、砷、铜、镍、铝等元素的分析方法.方法采用航空煤油为稀释剂,按照油/溶剂（质量比）1/9加以稀释后直接进人IC P - M S仪器分析,采用钇、铍混合内标来补偿仪器...目的采用加氧附件-有机进样系统建立了 IC P - M S 直接进样测定食用油中铅、砷、铜、镍、铝等元素的分析方法.方法采用航空煤油为稀释剂,按照油/溶剂（质量比）1/9加以稀释后直接进人IC P - M S仪器分析,采用钇、铍混合内标来补偿仪器信号漂移和基体效应.结果方法检出限：铅为 0.09μg/kg、砷为 0.07 pg/kg、铜为 0.1μg/kg、镍为 0.11 μg/kg、铝为 0.55μg/kg; 相对标准偏差〈5 % ; 加标回收率在9 5 % - 105 %之间.结论该研究所建立的方法适用于食用油等有机样品中重金属元素的检测分析.展开更多
In this work,the nano-g-C_(3)N_(4)/Ui O-66-NH_(2)composite was prepared by one-step solvothermal method.The as-prepared composite was characterized by scanning electron microscopy,Brunner-Emmet-Teller measurement,ener...In this work,the nano-g-C_(3)N_(4)/Ui O-66-NH_(2)composite was prepared by one-step solvothermal method.The as-prepared composite was characterized by scanning electron microscopy,Brunner-Emmet-Teller measurement,energy dispersive spectrometer,X-ray diffraction,and Fourier transform infrared spectroscopy.By using nano-g-C_(3)N_(4)/Ui O-66-NH_(2)composite as sorbent,a dispersive solid-phase extraction coupled with high-performance liquid chromatography was developed to sensitive analysis of food colorants including tartrazine,amaranth,carmine,sunset yellow,allura red and bright blue.The experiment parameters including the amount of sorbent,adsorption time,the p H of adsorption solution,desorption time,desorption solvent,the p H of desorption solution as well as the proportion between desorption solvent and buffer solvent were investigated.Under the optimized conditions,the limits of detection(S/N=3) and limits of quantitation (S/N=10) were determined in the ranges of 0.08-0.8 and 0.2-2.0 ng/m L,respectively.With the developed sample pretreatment method,carmine and brilliant blue were determined from blueberry juice by HPLC-DAD.The contents were calculated as 1.53μg/m L and0.17μg/mL,respectively.展开更多
文摘目的采用加氧附件-有机进样系统建立了 IC P - M S 直接进样测定食用油中铅、砷、铜、镍、铝等元素的分析方法.方法采用航空煤油为稀释剂,按照油/溶剂（质量比）1/9加以稀释后直接进人IC P - M S仪器分析,采用钇、铍混合内标来补偿仪器信号漂移和基体效应.结果方法检出限：铅为 0.09μg/kg、砷为 0.07 pg/kg、铜为 0.1μg/kg、镍为 0.11 μg/kg、铝为 0.55μg/kg; 相对标准偏差〈5 % ; 加标回收率在9 5 % - 105 %之间.结论该研究所建立的方法适用于食用油等有机样品中重金属元素的检测分析.
基金sponsored by the National Nature Science Foundation of China (No.22076038)Natural Science Foundation of Henan (No.202300410044)。
文摘In this work,the nano-g-C_(3)N_(4)/Ui O-66-NH_(2)composite was prepared by one-step solvothermal method.The as-prepared composite was characterized by scanning electron microscopy,Brunner-Emmet-Teller measurement,energy dispersive spectrometer,X-ray diffraction,and Fourier transform infrared spectroscopy.By using nano-g-C_(3)N_(4)/Ui O-66-NH_(2)composite as sorbent,a dispersive solid-phase extraction coupled with high-performance liquid chromatography was developed to sensitive analysis of food colorants including tartrazine,amaranth,carmine,sunset yellow,allura red and bright blue.The experiment parameters including the amount of sorbent,adsorption time,the p H of adsorption solution,desorption time,desorption solvent,the p H of desorption solution as well as the proportion between desorption solvent and buffer solvent were investigated.Under the optimized conditions,the limits of detection(S/N=3) and limits of quantitation (S/N=10) were determined in the ranges of 0.08-0.8 and 0.2-2.0 ng/m L,respectively.With the developed sample pretreatment method,carmine and brilliant blue were determined from blueberry juice by HPLC-DAD.The contents were calculated as 1.53μg/m L and0.17μg/mL,respectively.
