小中大回复 #1 linger0824 的帖子
楼主的这个化合物，盐酸坦索罗辛（Tamsulosin hydrochloride），有很多文献报道的吧？
看文献多用硫化-环糊精，楼主是重复不出来文献的方法呢？还是因为没有硫化-环糊精，亦或者是想做方法学改进？
羧甲基环糊精，如CM-β-CD (carboxymethyl-β-CD)有试验过吗？是否有分离效果？
Enantiomeric purity determination of tamsulosin by capillary electrophoresis using cyclodextrins and a polyacrylamide-coated capillary
Il Farmaco
Volume 60, Issue 10, October 2005, Pages 834-839
cuturl('http://www.sciencedirect.com/science?_ob=ArticleURL&_udi=B6VJ8-4H0S1N5-2&_user=10&_coverDate=10%2F31%2F2005&_rdoc=1&_fmt=high&_orig=search&_origin=search&_sort=d&_docanchor=&view=c&_searchStrId=1540683367&_rerunOrigin=google&_acct=C000050221&_version=1&_urlVersion=0&_userid=10&md5=842325b0d4624bbabfef58b773952b92&searchtype=a')
Abstract
The chiral separation of racemic tamsulosin hydrochloride (TH) was carried out using cyclodextrin (CD)-mediated capillary electrophoresis (CE) with DAD at 200 nm. The best separation of enantiomers of the studied compound was achieved at 20 kV with 30 cm × 50 μm I.D. polyacrylamide (PAA)-coated fused-silica capillary (effective length 20 cm) and running buffer with sulfated-β-CD (S-β-CD) as chiral selector. Other selected native or derivatized CDs were also tested: β-CD (5, 15 mmol l−1), carboxymethyl-β-CD (5, 30 mmol l−1), dimethyl-β-CD (15 mmol l−1) and hydroxypropyl-β-CD (5, 30 mmol l−1). Several parameters such as capillary pretreatment, buffer type and concentration, pH of background electrolyte, methanol content, separation temperature and voltage, were optimized. The excellent baseline separation of chiral TH was successfully achieved within 12 min using 100 mmol l−1 phosphate buffer with pH 2.5 containing 1.7 mmol l−1 S-β-CD. Rectilinear calibration range was 50.0–500.0 μmol l−1 of each enantiomer (r = 0.9993–0.9996).
The method was applied to the assay of R-TH in Omnic, capsules (nominal content 0.4 mg per capsule) with R.S.D. 2.75% (n = 6), recovery 99.3–101.7% and it was suitable for the chiral purity control of the active enantiomer in the pharmaceutical.
个人更喜欢chiral HPL， 呵呵
