Determination of Enantiomeric Purity of GSK962040 Based on Liquid Chromatography Using Chiral Stationary Phase Combined with a Pre-column Derivatization Procedure
Determination of Enantiomeric Purity of GSK962040 Based on Liquid Chromatography Using Chiral Stationary Phase Combined with a Pre-column Derivatization Procedure
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基于手性固定相结合柱前衍生化程序的液相色谱法测定 GSK962040 对映体纯度
DOI：
10.1007/s10337-017-3338-7
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发表时间：
2017-06
期刊：
影响因子：
1.7
通讯作者：
Yiwen Zhang
中科院分区：
文献类型：
--
作者：
Tinghong Ye;Mengya Liao;Mingxing Hu;Yongmei Xie;Yiwen Zhang
建立了一种灵敏、准确的液相色谱法，并进一步验证了该方法用于测定GSK 962040的对映体纯度。在分离之前，进行柱前衍生化程序。使用Chiralpak AD-H（250 × 4.6 mm;粒度5 μm）色谱柱，以正己烷：2-丙醇（85：15 v/v）作为移动的相，流速为1 mL min−1，在15 min内实现基线分离，分离度高于1.9。随后用UV检测器在260 nm处检测洗脱的分析物。考察了移动的组分和温度对对映体选择性及对映体拆分的影响。在4 ~ 200 μg mL−1（n= 8）浓度范围内绘制标准曲线，回收率在98.15 ~ 101.48%之间，相对标准偏差（RSD）小于1.42%。Boc-GSK 962040的LOD和LOQ分别为1.23和4.15 μg mL− 1，其对映异构体的LOD和LOQ分别为1.38和4.76 μg mL−1。通过分析具有不同对映体比例的GSK 962040的散装样品，对所开发的方法进行了评价和验证。结果表明，该方法准确、灵敏、稳定，可用于真实的分析。
A sensitive and accurate LC method was developed and further validated for the determination of enantiomeric purity of GSK962040. Before separation, a pre-column derivatization procedure was performed. Baseline separation with a resolution higher than 1.9 was accomplished within 15 min using a Chiralpak AD-H (250 × 4.6 mm; particle size 5 μm) column, withn-hexane: 2-propanol (85:15v/v) as mobile phase at a flow rate of 1 mL min−1. The eluted analytes were subsequently detected with a UV detector at 260 nm. The effects of mobile phase components and temperature on enantiomeric selectivity as well as resolution of enantiomers were thoroughly investigated. The calibration curves were plotted within the concentration range between 4 and 200 μg mL−1(n= 8), and recoveries between 98.15 and 101.48% were obtained, with relative standard deviation (RSD) lower than 1.42%. The LOD and LOQ for the Boc-GSK962040 were 1.23 and 4.15 μg mL−1and for its enantiomer were 1.38 and 4.76 μg mL−1, respectively. The developed method was also evaluated and validated by analyzing bulk samples with different enantiomeric ratios of GSK962040. It was demonstrated that the method was accurate, robust and sensitive, and also had practical utilities for real analysis.
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影响因子：
7.3
作者：
Hellstrom, Per M.;Tack, Jan;Dukes, George E.
通讯作者：
Dukes, George E.
影响因子：
3.5
作者：
R. Hobson;A. Farmer;O. Dewit;M. O'Donnell;K. Hacquoil;D. Robertson;M. Barton;G. Dukes
通讯作者：
R. Hobson;A. Farmer;O. Dewit;M. O'Donnell;K. Hacquoil;D. Robertson;M. Barton;G. Dukes
影响因子：
3.4
作者：
R. Nageswara Rao;A. Narasa Raju;D. Nagaraju
通讯作者：
R. Nageswara Rao;A. Narasa Raju;D. Nagaraju
DOI：
10.1016/s0378-4347(00)00267-x
发表时间：
2000-08
期刊：
Journal of chromatography. B, Biomedical sciences and applications
影响因子：
--
作者：
Q. Sun;S. Olesik
通讯作者：
Q. Sun;S. Olesik
影响因子：
3.5
作者：
Gareth J. Sanger;S. Westaway;A. A. Barnes-A.;David T. MacPherson;Alison I. Muir;E. Jarvie;V. N. Bolton;Selim Cellek;Erik Näslund;Per M. Hellström;Richard A. Borman;W. P. Unsworth;Kim L. Matthews;Kevin Lee
通讯作者：
Gareth J. Sanger;S. Westaway;A. A. Barnes-A.;David T. MacPherson;Alison I. Muir;E. Jarvie;V. N. Bolton;Selim Cellek;Erik Näslund;Per M. Hellström;Richard A. Borman;W. P. Unsworth;Kim L. Matthews;Kevin Lee