Performance and lifetime of slurry packed capillary columns for high performance liquid chromatography

2014 ◽  
Vol 68 (1) ◽  
Author(s):  
Martin Franc ◽  
Jiří Vojta ◽  
Jana Sobotníková ◽  
Pavel Coufal ◽  
Zuzana Bosáková

AbstractFused silica capillary columns of the internal diameter of 320 μm were packed with the Nucleosil C18 stationary phase of 5 μm using the slurry packing method. The time of the bed compaction phase, packing pressure, and the use of ultrasound varied to study their influence on the column performance. Van Deemter curves were measured and separation impedance values were calculated in order to assess both separation efficiency and kinetic performance of the columns. Selected columns were tested again after nine months to evaluate the stability of their beds. Separation efficiencies of all columns were similar, but a major difference, caused by the use of ultrasound, was observed in the bed stability. Columns sonicated for 25 minutes during the bed compaction phase exhibited unchanged performance in the course of several months, while the performance of non-sonicated columns decreased.

1983 ◽  
Vol 279 ◽  
pp. 99-102 ◽  
Author(s):  
M. Verzele ◽  
F. David ◽  
M. Van Roelenbosch ◽  
G. Diricks ◽  
P. Sandra

1983 ◽  
Vol 66 (4) ◽  
pp. 1029-1038
Author(s):  
Hing-Biu Lee ◽  
Alfred S Y Chau

Abstract A gas-liquid chromatographic (GLC) procedure is described for the identification of 32 substituted phenols including all 19 chlorophenols and the 11 U.S. Environmental Protection Agency consent decree phenols. This method involves a simple and reproducible derivatization step which forms stable phenol PFB ethers for which the electron capture detector is highly sensitive. GLC retention time data of the derivatives on 6 packed and fused silica capillary columns (FSCC) are reported. The detection limits of all chloro-, alkyl- and mono-nitrophenols studied are between 0.5 and 5 pg injected for an FSCC. The high resolution of these capillary columns makes this method isomer-specific. The derivatization procedure also eliminates the sensitivity, tailing, and resolution problems commonly encountered in other gas chromatographic methods on underivatized phenols.


2012 ◽  
Vol 2012 ◽  
pp. 1-10 ◽  
Author(s):  
Sanjay A. Jadhav ◽  
Shashikant B. Landge ◽  
Navanath C. Niphade ◽  
Saroj R. Bembalkar ◽  
Vijayavitthal T. Mathad

A stability-indicating method has been developed and validated for the quantitative determination of memantine hydrochloride and its nonchromophoric impurities in drug substance and drug product using gas chromatography coupled with flame ionization detector (GC-FID). The stability-indicating nature of the method has been proved by establishing peak purity and confirming the mass balance of all samples by subjecting them to stress conditions like hydrolysis, oxidation, photolysis, and thermal degradation studies. The chromatographic separation was performed on a fused silica capillary (HP-5, 30 meter, 0.32 mm and 0.25 μm film thickness) column. The method validation results indicate that the method has acceptable specificity, accuracy, linearity, precision, robustness, and high sensitivity with detection limits and quantitation limits ranging from 0.001% to 0.01% and 0.004% to 0.03%, respectively. The effectiveness of the technique was demonstrated by analysis of different bulk sample of Memantine hydrochloride. The proposed GC-FID method was also found to be specific and selective for the analysis of commercial formulation samples.


Sign in / Sign up

Export Citation Format

Share Document