scholarly journals HPLC Separation of Diastereomers: Chiral Molecular Tools Useful for the Preparation of Enantiopure Compounds and Simultaneous Determination of Their Absolute Configurations

Molecules ◽  
2016 ◽  
Vol 21 (10) ◽  
pp. 1328 ◽  
Author(s):  
Nobuyuki Harada
2009 ◽  
Vol 92 (4) ◽  
pp. 1089-1094
Author(s):  
Tai-Li Tsou ◽  
Chiu-Wey Lee ◽  
Hsian-Jenn Wang ◽  
Ya-Chung Cheng ◽  
Yu-Tien Liu ◽  
...  

Abstract A new HPLC method has been developed and validated for the simultaneous determination of ticarcillin (TIC) and clavulanic acid (CA) in pharmaceutical formulations. The HPLC separation was achieved on a -cyclodextrin column (Cyclobond I, 250 4.6 mm, 5 mm) with methanol16 mM pH 6.0 ammonium acetate buffer (50 + 50, v/v) mobile phase at a flow rate of 0.8 mL/min. Detection was at 220 nm. Validation of the method was performed by evaluating specificity, robustness, accuracy, and precision. The calibration curves were linear in the range of 1100 g/mL for CA and 2200 g/mL for TIC. The LOQs based on the standard regression lines were 0.42 and 1.42 g/mL for CA and TIC, respectively, and the LOD were 0.14 and 0.47 g/mL, respectively. Total recoveries of synthetic mixtures (CA:TIC = 1:10, 1:15, and 1:30) were 99.25100.99 for CA and 99.54100.82 for TIC. Compared with the U.S. Pharmacopeia method, the proposed method has the advantage of a relatively low flow rate and short analysis time. The proposed method was successfully applied for the simultaneous determination of these two drugs in sterilized H2O and 5 dextrose injection solutions.


ChemInform ◽  
2005 ◽  
Vol 36 (17) ◽  
Author(s):  
Yusuke Kasai ◽  
Junpei Naito ◽  
Shunsuke Kuwahara ◽  
Masataka Watanabe ◽  
Akio Ichikawa ◽  
...  

2011 ◽  
Vol 39 (05) ◽  
pp. 1043-1060 ◽  
Author(s):  
Cheng-Cheng Cai ◽  
Ma-Cheng Yan ◽  
Hui Xie ◽  
Sheng-Li Pan

Piper is a genus that is recently valued for the treatment of central nervous system diseases. The major constituents, amides and lignans, are responsible for the antinociceptive and antidepressant activities. This study developed a RP-HPLC-UV method for the simultaneous determination of eight amides and two lignans in twelve different species of Piper. HPLC separation was accomplished on a C18 analytical column (5 μm, 250 mm × 4.6 mm, i.d.) with a gradient mobile phase consisting of acetonitrile and water at a flow rate of 1.0 ml/min. All the calibration curves showed good linear correlation coefficients (r > 0.9997) over the test ranges. The relative standard deviation of the current method was less than 2.90% for intra- and inter-day assays and the average recoveries were between 98.25% and 103.08%. The HPLC method established is appropriate for quality control purposes and allows for the differentiation of Piper species.


2011 ◽  
Vol 94 (1) ◽  
pp. 150-158 ◽  
Author(s):  
Farhan Ahmed Siddiqui ◽  
M Saeed Arayne ◽  
Najma Sultana ◽  
Faiza Qureshi

Abstract A method is described for the simultaneous determination of paracetamol, tizanidine, and diclofenac in mixtures. The method was based on HPLC separation of the three drugs followed by UV detection at 254 nm. The separation was carried out on a Hypersil ODS, C18 (250 × 4.6 mm id, 10 μm particle size) column using the mobile phase aqueous 0.2% ammonium carbonate–methanol (60 + 40, v/v) at a flow rate of 1 mL/min. The linear regression analysis data were used for the regression curve in the range of 170–10,000 ng/mL for paracetamol, 120–10,000 ng/mL for tizanidine, and 20–10,000 ng/mL for diclofenac. No chromatographic interference from tablet excipients was found. In order to check the selectivity of the proposed method, degradation studies were carried out using hydrolysis (acid, basic, and neutral), thermolysis, and oxidation. The developed method, after being validated in terms of precision, robustness, recovery, LOD, and LOQ, was successively applied to the analysis of pharmaceutical formulations and human serum.


1978 ◽  
Vol 48 ◽  
pp. 287-293 ◽  
Author(s):  
Chr. de Vegt ◽  
E. Ebner ◽  
K. von der Heide

In contrast to the adjustment of single plates a block adjustment is a simultaneous determination of all unknowns associated with many overlapping plates (star positions and plate constants etc. ) by one large adjustment. This plate overlap technique was introduced by Eichhorn and reviewed by Googe et. al. The author now has developed a set of computer programmes which allows the adjustment of any set of contemporaneous overlapping plates. There is in principle no limit for the number of plates, the number of stars, the number of individual plate constants for each plate, and for the overlapping factor.


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