Different fused-core stationary phase chemistries（C18,Amide,Phenyl-hexyl and Peptide ES-C18） were used for the analysis of 21 structurally representative model peptides.In addition,the effects of the mobile phase co...Different fused-core stationary phase chemistries（C18,Amide,Phenyl-hexyl and Peptide ES-C18） were used for the analysis of 21 structurally representative model peptides.In addition,the effects of the mobile phase composition（ACN or MeOH as organic modifier;formic acid or acetic acid,as acidifying component） on the column selectivity,peak shape and overall chromatographic performance were evaluated.The RP-amide column,combined with a formic acid-acetonitrile based gradient system,performed as best.A peptide reversed-phase retention model is proposed,consisting of 5 variables：log SumAA,log Sv,clog P,log nHDon and log nHAcc.Quantitative structure-retention relationship（QSRR） models were constructed for 16 different chromatographic systems.The accuracy of this peptide retention model was demonstrated by the comparison between predicted and experimentally obtained retention times,explaining on average 86% of the variability.Moreover,using an external set of 5 validation peptides,the predictive power of the model was also demonstrated.This peptide retention model includes the novel in-silico calculated amino acid descriptor,AA,which was calculated from log P,3D-MoRSE,RDF and WHIM descriptors.展开更多
For several years, near-infrared spectroscopy (NIRS) has become an analytical technique of great interest for the pharmaceutical industry, particularly for the non-destructive analysis of dosage forms. The goal of thi...For several years, near-infrared spectroscopy (NIRS) has become an analytical technique of great interest for the pharmaceutical industry, particularly for the non-destructive analysis of dosage forms. The goal of this study is to show the capacity of this new technique to assay the active ingredient in low-dosage tablets. NIR spectroscopy is a rapid, non-destructive technique and does not need any sample preparation. A prediction model was built by using a partial least square regression fit method. The NIR assay was performed by transmission. The results obtained by NIR spectroscopy were compared with the conventional HPLC method for Montelukast tablets produced by Sigma pharmaceutical corp. The study showed that Montelukast tablets can be individually analyzed by NIR with high accuracy. It was shown that the variability of this new tech- nique is less important than that of the conventional method which is the HPLC with UV detection.展开更多
目的:建立一种手持式近红外光谱技术与正交投影偏最小二乘法(orthogonal projection partial least squares,OPLS)相结合的快速检测姜黄丸原料混合物中姜黄素含量的方法。方法:取姜黄、炒蒺藜饮片,分别粉碎过筛,按照不同比例混合均匀,制...目的:建立一种手持式近红外光谱技术与正交投影偏最小二乘法(orthogonal projection partial least squares,OPLS)相结合的快速检测姜黄丸原料混合物中姜黄素含量的方法。方法:取姜黄、炒蒺藜饮片,分别粉碎过筛,按照不同比例混合均匀,制备26个样本;采用HPLC方法测定样品中姜黄素含量,以测定值为标签值(Y),手持式近红外光谱仪分别采集每批样品的近红外光谱数据5次取平均值作为近红外基础数据(X,n=26);利用SIMCA 14.1软件进行光谱数据的预处理,利用k折交叉验证方法建立姜黄丸的正交投影偏最小二乘法(OPLS)定量校正模型Y=M(X)。结果:预测Y值与实测Y值OPLS模型回归方程的决定系数R2为0.9893,RMSECV为0.0751;采用Permutation(置换检验)对模型进行内部验证,结果发现模型没有出现过拟合,模型预测效果良好。结论:利用手持式近红外光谱仪可以实现对姜黄丸原料混合物的快速、无损检测。展开更多
大株红景天为景天科植物大株红景天的干燥根和根茎,主产于西藏、四川、青海及云南等地,为大株红景天注射液、大株红景天片和大株红景天胶囊等中成药制剂的主要原料,应用较为广泛.本研究以乙腈-0.1%甲酸为流动相进行梯度洗脱,检测波长分...大株红景天为景天科植物大株红景天的干燥根和根茎,主产于西藏、四川、青海及云南等地,为大株红景天注射液、大株红景天片和大株红景天胶囊等中成药制剂的主要原料,应用较为广泛.本研究以乙腈-0.1%甲酸为流动相进行梯度洗脱,检测波长分别为275和360 nm,采用高效液相色谱(high performance liquid chromatography,HPLC)法同时测定大株红景天中没食子酸、酪醇、熊果苷、红景天苷、表儿茶素、儿茶素、咖啡酸、对香豆酸、草质素、红景天素、山萘酚和槲皮素含量;同时对多指标成分含量检测结果进行主成分分析(principal component analysis,PCA)、正交偏最小二乘法-判别分析(orthogonal partial least squares-discriminant analysis,OPLS-DA),并建立熵权优劣解距离法(Technique for order preference by similarity to an ideal solution,TOPSIS)模型,探索HPLC多成分定量及化学计量学、熵权TOPSIS模型在大株红景天质量评价中的应用.结果显示HPLC多成分定量检测方法方法学符合《中国药典》规定;化学计量学分析结果显示16批大株红景天聚为3类,提示酪醇、红景天苷、红景天素、没食子酸和熊果苷是影响大株红景天产品质量的主要潜在标志物;熵权TOPSIS法最优解的欧氏贴近度(C_(i))为0.2251-0.7479,16批大株红景天呈现一定产地差异.建立的HPLC多成分定量及化学计量学、熵权TOPSIS模型操作便捷,结果准确,可用于大株红景天整体质量的综合评价.展开更多
基金funded by a Ph.D.grant of "Institute for the Promotion of Innovation through Science and Technology in Flanders(IWT-Vlaanderen)"(No.091241 for MD and 073402 for SVD)the Special Research Fund of the Ghent University (Grant no.BOF 01J22510 for EW and BOF 01D38811 for SS)
文摘Different fused-core stationary phase chemistries（C18,Amide,Phenyl-hexyl and Peptide ES-C18） were used for the analysis of 21 structurally representative model peptides.In addition,the effects of the mobile phase composition（ACN or MeOH as organic modifier;formic acid or acetic acid,as acidifying component） on the column selectivity,peak shape and overall chromatographic performance were evaluated.The RP-amide column,combined with a formic acid-acetonitrile based gradient system,performed as best.A peptide reversed-phase retention model is proposed,consisting of 5 variables：log SumAA,log Sv,clog P,log nHDon and log nHAcc.Quantitative structure-retention relationship（QSRR） models were constructed for 16 different chromatographic systems.The accuracy of this peptide retention model was demonstrated by the comparison between predicted and experimentally obtained retention times,explaining on average 86% of the variability.Moreover,using an external set of 5 validation peptides,the predictive power of the model was also demonstrated.This peptide retention model includes the novel in-silico calculated amino acid descriptor,AA,which was calculated from log P,3D-MoRSE,RDF and WHIM descriptors.
文摘For several years, near-infrared spectroscopy (NIRS) has become an analytical technique of great interest for the pharmaceutical industry, particularly for the non-destructive analysis of dosage forms. The goal of this study is to show the capacity of this new technique to assay the active ingredient in low-dosage tablets. NIR spectroscopy is a rapid, non-destructive technique and does not need any sample preparation. A prediction model was built by using a partial least square regression fit method. The NIR assay was performed by transmission. The results obtained by NIR spectroscopy were compared with the conventional HPLC method for Montelukast tablets produced by Sigma pharmaceutical corp. The study showed that Montelukast tablets can be individually analyzed by NIR with high accuracy. It was shown that the variability of this new tech- nique is less important than that of the conventional method which is the HPLC with UV detection.
文摘大株红景天为景天科植物大株红景天的干燥根和根茎,主产于西藏、四川、青海及云南等地,为大株红景天注射液、大株红景天片和大株红景天胶囊等中成药制剂的主要原料,应用较为广泛.本研究以乙腈-0.1%甲酸为流动相进行梯度洗脱,检测波长分别为275和360 nm,采用高效液相色谱(high performance liquid chromatography,HPLC)法同时测定大株红景天中没食子酸、酪醇、熊果苷、红景天苷、表儿茶素、儿茶素、咖啡酸、对香豆酸、草质素、红景天素、山萘酚和槲皮素含量;同时对多指标成分含量检测结果进行主成分分析(principal component analysis,PCA)、正交偏最小二乘法-判别分析(orthogonal partial least squares-discriminant analysis,OPLS-DA),并建立熵权优劣解距离法(Technique for order preference by similarity to an ideal solution,TOPSIS)模型,探索HPLC多成分定量及化学计量学、熵权TOPSIS模型在大株红景天质量评价中的应用.结果显示HPLC多成分定量检测方法方法学符合《中国药典》规定;化学计量学分析结果显示16批大株红景天聚为3类,提示酪醇、红景天苷、红景天素、没食子酸和熊果苷是影响大株红景天产品质量的主要潜在标志物;熵权TOPSIS法最优解的欧氏贴近度(C_(i))为0.2251-0.7479,16批大株红景天呈现一定产地差异.建立的HPLC多成分定量及化学计量学、熵权TOPSIS模型操作便捷,结果准确,可用于大株红景天整体质量的综合评价.
