目的建立高效阴离子交换色谱-脉冲安培法(high-performance anion exchange chromatography with pulsed ampe-rometric detector,HPAEC-PAD)检测以吸附无细胞百(三组分)白破(diphtheria,tetanus and component acellular pertu-ssis va...目的建立高效阴离子交换色谱-脉冲安培法(high-performance anion exchange chromatography with pulsed ampe-rometric detector,HPAEC-PAD)检测以吸附无细胞百(三组分)白破(diphtheria,tetanus and component acellular pertu-ssis vaccine,DTacP)为基础的联合疫苗中甘油含量,并对方法进行验证和初步应用,以期为联合疫苗中甘油的检测及质量控制提供更好的手段.方法离心去除样品中氢氧化铝佐剂,上清过0.22μm膜后,采用MA-1色谱柱分离,使用安培检测器检测,外标法建立标准曲线.对方法进行专属性、线性、检测限(limit of detection,LOD)和定量限(limit of quantitation,LOQ)、准确度、精密度及耐用性验证.采用建立的方法检测9批次以DTacP为基础的联合疫苗的甘油含量.结果乙二醇、甘油和核糖醇可有效分离,方法专属性较强;在0.9~28.7μg/mL浓度范围内,甘油参考品质量浓度与峰面积呈良好的线性关系,R2均>0.999;方法的LOD为110 ng/mL,LOQ为500 ng/mL;该方法检测高(25.0μg/mL)、中(15μg/mL)、低(1.5μg/mL)质量浓度甘油参考品的加标回收率均在95%~105%之间;精密度验证的相对标准偏差(relative standard deviation,RSD)均<2%;改变流速(0.4→0.3 mL/min)、柱温(30→32℃)、流动相浓度(450→580 mmol/L),检测结果差异小.建立的方法可准确检测DTacP、吸附无细胞百(三组分)白破灭活脊髓灰质炎联合疫苗(DTacP-sIPV)和吸附无细胞百(三组分)白破灭活脊髓灰质炎与b型流感嗜血杆菌(结合)联合疫苗(DTacP-sIPV-Hib)中的甘油含量,RSD最大仅为0.78%.结论建立的HPAEC-PAD法专属性、线性、准确度、精密度及耐用性良好,可定量分析DTacP系列联合疫苗中的甘油含量,为DTacP系列联合疫苗的质量控制提供了更好的手段.展开更多
Researching novel hydrogen evolution reaction(HER)catalysts with enhanced electrocatalytic activity,excellent stability,and cost-efficiency is of great significance for the large-scale hydrogen production from industr...Researching novel hydrogen evolution reaction(HER)catalysts with enhanced electrocatalytic activity,excellent stability,and cost-efficiency is of great significance for the large-scale hydrogen production from industrial electrolysis technology.We report the preparation of hierarchical mesoporous-Pt nanoparticles(HM-Pt NPs)with coral-like rough surface morphologies using environmental friendly and biocompatible fucoidan(Fu)biopolymer as a surface engineering compound and its application to electrocatalysts for water-splitting.The designed HM-Pt NPs yields better mass activity of electrocatalysts compared to a commercial Pt/C.HM-Pt NPs showed an overpotential of 33 mV at 10 mA cm-2 for the HER in 0.5 MH2SO4,which was highly comparable to that of the commercial Pt/C catalysts(29 mV).However,the amount of HM-Pt NPs loaded in glassy carbon electrode(0.033 mg mL-1)was approximately 20 times lower than that of the commercial Pt/C(0.64 mg mL-1.The HM-Pt NPs also maintained high catalytic stability with a consistent HER current density after 1000 continuous operation.The excellent HER performance is attributed to the improved electrochemical surface area,highly porous structure,and good surface wettability of the HM-Pt NPs,which results in enhanced electrocatalytic activity,decreased resistance at the electrode/electrolyte interface,and facile penetration of the electrolytes inside the electrode.展开更多
文摘目的建立高效阴离子交换色谱-脉冲安培法(high-performance anion exchange chromatography with pulsed ampe-rometric detector,HPAEC-PAD)检测以吸附无细胞百(三组分)白破(diphtheria,tetanus and component acellular pertu-ssis vaccine,DTacP)为基础的联合疫苗中甘油含量,并对方法进行验证和初步应用,以期为联合疫苗中甘油的检测及质量控制提供更好的手段.方法离心去除样品中氢氧化铝佐剂,上清过0.22μm膜后,采用MA-1色谱柱分离,使用安培检测器检测,外标法建立标准曲线.对方法进行专属性、线性、检测限(limit of detection,LOD)和定量限(limit of quantitation,LOQ)、准确度、精密度及耐用性验证.采用建立的方法检测9批次以DTacP为基础的联合疫苗的甘油含量.结果乙二醇、甘油和核糖醇可有效分离,方法专属性较强;在0.9~28.7μg/mL浓度范围内,甘油参考品质量浓度与峰面积呈良好的线性关系,R2均>0.999;方法的LOD为110 ng/mL,LOQ为500 ng/mL;该方法检测高(25.0μg/mL)、中(15μg/mL)、低(1.5μg/mL)质量浓度甘油参考品的加标回收率均在95%~105%之间;精密度验证的相对标准偏差(relative standard deviation,RSD)均<2%;改变流速(0.4→0.3 mL/min)、柱温(30→32℃)、流动相浓度(450→580 mmol/L),检测结果差异小.建立的方法可准确检测DTacP、吸附无细胞百(三组分)白破灭活脊髓灰质炎联合疫苗(DTacP-sIPV)和吸附无细胞百(三组分)白破灭活脊髓灰质炎与b型流感嗜血杆菌(结合)联合疫苗(DTacP-sIPV-Hib)中的甘油含量,RSD最大仅为0.78%.结论建立的HPAEC-PAD法专属性、线性、准确度、精密度及耐用性良好,可定量分析DTacP系列联合疫苗中的甘油含量,为DTacP系列联合疫苗的质量控制提供了更好的手段.
基金the National Research Foundation of Korea(NRF)grant funded by the Korea government(MSIP)(NRF-2019R1C1C1010283 and NRF-2019R1C1C1002305)。
文摘Researching novel hydrogen evolution reaction(HER)catalysts with enhanced electrocatalytic activity,excellent stability,and cost-efficiency is of great significance for the large-scale hydrogen production from industrial electrolysis technology.We report the preparation of hierarchical mesoporous-Pt nanoparticles(HM-Pt NPs)with coral-like rough surface morphologies using environmental friendly and biocompatible fucoidan(Fu)biopolymer as a surface engineering compound and its application to electrocatalysts for water-splitting.The designed HM-Pt NPs yields better mass activity of electrocatalysts compared to a commercial Pt/C.HM-Pt NPs showed an overpotential of 33 mV at 10 mA cm-2 for the HER in 0.5 MH2SO4,which was highly comparable to that of the commercial Pt/C catalysts(29 mV).However,the amount of HM-Pt NPs loaded in glassy carbon electrode(0.033 mg mL-1)was approximately 20 times lower than that of the commercial Pt/C(0.64 mg mL-1.The HM-Pt NPs also maintained high catalytic stability with a consistent HER current density after 1000 continuous operation.The excellent HER performance is attributed to the improved electrochemical surface area,highly porous structure,and good surface wettability of the HM-Pt NPs,which results in enhanced electrocatalytic activity,decreased resistance at the electrode/electrolyte interface,and facile penetration of the electrolytes inside the electrode.
