PMID- 22865752
OWN - NLM
STAT- MEDLINE
DCOM- 20121203
LR  - 20191210
IS  - 1615-9314 (Electronic)
IS  - 1615-9306 (Linking)
VI  - 35
IP  - 15
DP  - 2012 Aug
TI  - HPLC enantioseparation of alkaloid malacitanine using fluorimetric/polarimetric 
      detection.
PG  - 1863-8
LID - 10.1002/jssc.201200275 [doi]
AB  - This work reports two methods developed for the separation and determination of 
      the enantiomers of the new alkaloid malacitanine (MLC) and the determination of 
      the enantiomeric purity in mixtures. First, the isomers were separated using a 
      Chirex 3020 (250 mm x 4.6 mm, 5 mum) chiral column with a mobile phase of 
      cyclohexane-1,2-dichloroethane-ethanol-trifluoroacetic acid (64:30:6:0.6, 
      v/v/v/v) at a flow rate of 1 mL/min and fluorimetric detection. Obtained 
      retention times were 12.4 and 15.9 min (+ and -) with a resolution Rs of 1.13. 
      Relative standard deviations (RSDs) were 2.5 and 2.4% at the 0.5-mug level (four 
      determinations). Second, a nonenantioselective procedure for the determination of 
      enantiomeric purity of MLC using a Lichrospher (R) Si-60 (250 mm x 5 mm, 5 mum) 
      normal phase with a mobile phase of 100% ethanol at a flow rate of 0.9 mL/min 
      coupled to two detectors in series, fluorimetric and polarimetric. RSD of 3.3% 
      was obtained. Calculated enantiomeric purity by chiral chromatography gave 48.6% 
      (-)-MLC in the near racemic product. Using polarimetric signal of the 
      nonseparated enantiomers and comparing the slopes of the calibration curves 
      (enantiomers) from the racemic product gave 47.8% (-)-MLC content. A study of 
      accuracy of (-)-MLC gave recoveries from 98.3 to 100.7%.
CI  - (c) 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
FAU - Garcia Sanchez, Francisco
AU  - Garcia Sanchez F
AD  - Department of Analytical Chemistry, Faculty of Science, University of Malaga, 
      Malaga, Spain. f_garcia@uma.es
FAU - Navas Diaz, Aurora
AU  - Navas Diaz A
FAU - Aguilar, Alfonso
AU  - Aguilar A
FAU - Medina Lama, Ignacio
AU  - Medina Lama I
FAU - Algarra, Manuel
AU  - Algarra M
LA  - eng
PT  - Evaluation Study
PT  - Journal Article
PL  - Germany
TA  - J Sep Sci
JT  - Journal of separation science
JID - 101088554
RN  - 0 (Alkaloids)
SB  - IM
MH  - Alkaloids/*chemistry/isolation & purification
MH  - Chromatography, High Pressure Liquid/*methods
MH  - Fluorometry/*methods
MH  - Stereoisomerism
EDAT- 2012/08/07 06:00
MHDA- 2012/12/10 06:00
CRDT- 2012/08/07 06:00
PHST- 2012/08/07 06:00 [entrez]
PHST- 2012/08/07 06:00 [pubmed]
PHST- 2012/12/10 06:00 [medline]
AID - 10.1002/jssc.201200275 [doi]
PST - ppublish
SO  - J Sep Sci. 2012 Aug;35(15):1863-8. doi: 10.1002/jssc.201200275.