Three novel amprolium HCl（AMP）-selective electrodes were investigated with 2-nitrophenyl octylether as a plasticiser in a polymeric matrix of polyvinyl chloride（PVC）. Sensor I was fabricated using potassium tetra...Three novel amprolium HCl（AMP）-selective electrodes were investigated with 2-nitrophenyl octylether as a plasticiser in a polymeric matrix of polyvinyl chloride（PVC）. Sensor I was fabricated using potassium tetrakis（4-chlorophenyl） borate（Tp ClPB） as a cationic exchanger without incorporation of an ionophore.Sensor Ⅱ used 2-hydroxy propyl β-cyclodextrin as an ionophore while sensor Ⅲ used p-tert-butylcalix[8]arene as an ionophore. The three proposed sensors showed Nernestian response slopes of 29.2±0.8,29.3±0.6 and 30.2±0.4 m V/decade over the concentration range from 10–6 to 10–2 mol L_（-1）,respectively. The proposed sensors displayed useful analytical characteristics for the determination of AMP in bulk powder, different pharmaceutical formulations, and chicken liver and in the presence of ethopabate. The proposed method was validated according to ICH guidelines for its linearity, accuracy,precision and robustness.展开更多
文摘Three novel amprolium HCl（AMP）-selective electrodes were investigated with 2-nitrophenyl octylether as a plasticiser in a polymeric matrix of polyvinyl chloride（PVC）. Sensor I was fabricated using potassium tetrakis（4-chlorophenyl） borate（Tp ClPB） as a cationic exchanger without incorporation of an ionophore.Sensor Ⅱ used 2-hydroxy propyl β-cyclodextrin as an ionophore while sensor Ⅲ used p-tert-butylcalix[8]arene as an ionophore. The three proposed sensors showed Nernestian response slopes of 29.2±0.8,29.3±0.6 and 30.2±0.4 m V/decade over the concentration range from 10–6 to 10–2 mol L_（-1）,respectively. The proposed sensors displayed useful analytical characteristics for the determination of AMP in bulk powder, different pharmaceutical formulations, and chicken liver and in the presence of ethopabate. The proposed method was validated according to ICH guidelines for its linearity, accuracy,precision and robustness.
文摘文章建立了一步式固相萃取净化、超高效液相色谱-串联质谱法测定动物性食品中氨丙啉残留量的方法。试样采用80%乙腈溶液(含0.2%甲酸)进行提取,PRi ME HLB(Hydrophi liclipophilic balanced)固相萃取柱净化,BEH HILIC(Hydrophilic interaction liquid chromatography)色谱柱分离,乙腈-含0.05%甲酸的5 mmol/L甲酸铵溶液为流动相进行梯度洗脱,电喷雾离子源正离子模式,多反应监测进行检测,基质匹配外标法定量。对提取溶剂、净化方式、色谱柱、流动相组成和质谱参数等重要因素进行了系统的考察。10种基质匹配标准曲线在0.25~100 ng/mL范围内,线性相关系数R2均大于0.99,检出限(Limit of detection,LOD)为2.0μg/kg,定量限(Limit of quantification,LOQ)为5.0μg/kg。在添加浓度水平5.0、50、500μg/kg条件下,回收率为86.10%~108.53%,相对标准偏差(n=6)为2.23%~8.42%。该方法采用一步式固相萃取净化,前处理简单、快速,避免溶剂转换、淋洗、洗脱、浓缩等多个处理过程,适用于鸡肉、牛肉、肝脏、肾脏、鸡蛋、脂肪和牛乳等动物性食品中氨丙啉残留的分析测定。
