Determination of AR-42 enantiomeric purity by HPLC on chiral stationary phase
Determination of AR-42 enantiomeric purity by HPLC on chiral stationary phase
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手性固定相 HPLC 测定 AR-42 对映体纯度
DOI：
10.1007/s13738-017-1130-0
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发表时间：
2017-05
影响因子：
2.4
通讯作者：
Yao Yuqin
中科院分区：
文献类型：
--
作者：
Fang Aiping;Zhang Yue;Shen Jiang;Sun Shijin;Zou Junyi;Yao Yuqin
建立了一种灵敏、准确的测定AR-42对映体纯度的高效液相色谱方法。色谱柱为CHIRALPAK AD柱(250 mm×24.6 mm，粒径5μm)，流动相为正己烷/异丙醇/二乙胺(75：25：0.1v/v/v)，流速为1mLmin−1。考察了流动相组成、温度和流速对对映体选择性和拆分的影响。−1的加标回收率为98.23%~101.87%，相对标准偏差小于1.31%，线性范围为0.001~0.5mg.mL.AR-42的检出限和定量限分别为0.39和1.28μg/mL−1，其对映体的检出限和定量限分别为0.36和1.19μg/mL−1。结果表明，该方法准确、可靠、灵敏，适用于AR-42对映体纯度的测定，特别适用于大样的分析。
A sensitive and accurate liquid chromatographic method for the determination of AR-42 enantiomeric purity has been developed and validated. Baseline separation with a resolution higher than 1.9 was accomplished within 10 min using a CHIRALPAK AD column (250 mm × 4.6 mm; particle size 5 μm) andn-hexane/2-propanol/diethylamine (75:25:0.1v/v/v) as mobile phase at a flow rate of 1 mL min−1. Eluted analytes were monitored by UV absorption at 260 nm. The effects of mobile phase components, temperature and flow rate on enantiomeric selectivity and resolution of enantiomers were investigated. Calibration curves were plotted within the concentration range between 0.001 and 0.5 mg mL−1(n= 10), and the recoveries between 98.23 and 101.87% were obtained, with relative standard deviation lower than 1.31%. Limit of detection and limit of quantitation for AR-42 were 0.39 and 1.28 μg mL−1and for its enantiomer were 0.36 and 1.19 μg mL−1, respectively. It was demonstrated that the developed method was accurate, robust and sensitive for the determination of enantiomeric purity of AR-42, especially for the analysis of bulk samples.
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DOI：
10.1073/pnas.1521827113
发表时间：
2016-03-15
影响因子：
11.1
作者：
Pattenden, Samantha G.;Simon, Jeremy M.;Davis, Ian J.
通讯作者：
Davis, Ian J.
影响因子：
11.5
作者：
Kulp, Samuel K.;Chen, Chang-Shi;Chen, Ching-Shih
通讯作者：
Chen, Ching-Shih
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
高效液相色谱分离手性固定相的开发
影响因子：
13.1
作者：
Tang, Mengling;Zhang, Jing;Liu, Weiping
通讯作者：
Liu, Weiping