The reintroduction of superficially porous particles has resulted in a leap forward for the separation performance in liquid chromatography. The underlying reasons for the higher efficiency of columns packed with thes...The reintroduction of superficially porous particles has resulted in a leap forward for the separation performance in liquid chromatography. The underlying reasons for the higher efficiency of columns packed with these particles are discussed. The performance of the newly introduced 5 p.m superficially porous particles is evaluated and compared to 2.7 pm superficially porous and 3.5 and 5 p.m fully porous columns using typical test compounds (alkylphenones) and a relevant pharmaceutical compound (impurity of amoxicillin). The 5 I.tm superficially porous particles provide a superior kinetic performance compared to both the 3.5 and 5 Ixm fully porous particles over the entire relevant range of separation conditions. The performance of the superficially porous particles, however, appears to depend strongly on retention and analyte properties, emphasizing the importance of comparing different columns under realistic conditions (high enough k) and using the compound of interest.展开更多
目的:建立基于单粒子光学传感技术的光阻法(LE/SPOS法),对脂肪乳静脉注射液中乳滴粒径大于5μm的尾部大粒子进行准确控制。方法:采用EXT模式(1.8-50μm),稀释流速60 m L·min-1,目标粒子数2000个·m L^-1,进样量0.98 m L...目的:建立基于单粒子光学传感技术的光阻法(LE/SPOS法),对脂肪乳静脉注射液中乳滴粒径大于5μm的尾部大粒子进行准确控制。方法:采用EXT模式(1.8-50μm),稀释流速60 m L·min-1,目标粒子数2000个·m L^-1,进样量0.98 m L,对仪器校正和检定后,分别对系统适用性、样品测定的精密度和中间精密度、回收率等方法学进行系统考察,并对多批乳剂样品进行检测。结果:5、10、25μm标准粒子测得的粒径大小和颗粒数均在标称值6%以内;不同PFAT5水平的脂肪乳样品测定的RSD≤5%,2台仪器测定的RSD〈10%,低、中、高3个PFAT5水平的5μm标准粒子平均回收率为100.5%,RSD〈2.0%(n=6);8批乳剂样品PFAT5测得值在0.010%-0.066%。结论:建立的光阻法操作简便,符合方法学考察要求,能够对脂肪乳静脉注射液中的PFAT5进行准确定量。展开更多
基金K.B.is a fellow of the Research Foundation Flanders (FWO Vlaanderen)
文摘The reintroduction of superficially porous particles has resulted in a leap forward for the separation performance in liquid chromatography. The underlying reasons for the higher efficiency of columns packed with these particles are discussed. The performance of the newly introduced 5 p.m superficially porous particles is evaluated and compared to 2.7 pm superficially porous and 3.5 and 5 p.m fully porous columns using typical test compounds (alkylphenones) and a relevant pharmaceutical compound (impurity of amoxicillin). The 5 I.tm superficially porous particles provide a superior kinetic performance compared to both the 3.5 and 5 Ixm fully porous particles over the entire relevant range of separation conditions. The performance of the superficially porous particles, however, appears to depend strongly on retention and analyte properties, emphasizing the importance of comparing different columns under realistic conditions (high enough k) and using the compound of interest.
文摘目的:建立基于单粒子光学传感技术的光阻法(LE/SPOS法),对脂肪乳静脉注射液中乳滴粒径大于5μm的尾部大粒子进行准确控制。方法:采用EXT模式(1.8-50μm),稀释流速60 m L·min-1,目标粒子数2000个·m L^-1,进样量0.98 m L,对仪器校正和检定后,分别对系统适用性、样品测定的精密度和中间精密度、回收率等方法学进行系统考察,并对多批乳剂样品进行检测。结果:5、10、25μm标准粒子测得的粒径大小和颗粒数均在标称值6%以内;不同PFAT5水平的脂肪乳样品测定的RSD≤5%,2台仪器测定的RSD〈10%,低、中、高3个PFAT5水平的5μm标准粒子平均回收率为100.5%,RSD〈2.0%(n=6);8批乳剂样品PFAT5测得值在0.010%-0.066%。结论:建立的光阻法操作简便,符合方法学考察要求,能够对脂肪乳静脉注射液中的PFAT5进行准确定量。