scholarly journals Desenvolvimento de um método analítico rápido e eficiente para a determinação de corticosteróides plasmáticos por injeção direta em coluna cromatográfica ISRP-C18 por CLAE.

2018 ◽  
Vol 35 (2) ◽  
pp. 51
Author(s):  
Eliane Aparecida Toledo-Pinto ◽  
Manoel Lima de Menezes ◽  
O. C. M. Pereira
Keyword(s):  
Analytical Method ◽  
Mobile Phase ◽  
High Efficiency ◽  
Direct Injection ◽  
Wave Length ◽  
Internal Surface ◽  
Previous Treatment ◽  
Ultraviolet Detector ◽  
On Line

The present work had as aim the development of simple an analytical method, fast efficient and the determination of corticosteroids (cortisone, corticosterone, acetate of hidrocortisone and acetate of dexametasone) in sanguine samples of rats using an isocratic system of liquid chromatography of high efficiency (CLAE) with ultraviolet detention. The methodinvolved direct injection of sanguine sample in a chromatographic column with internal surface of phase reverse (ISRP-C18), using the composed mobile phase for drain plug phosphate pH 4,0: acetonitrile (65:35 v/v). The detention the analytes was obtained using an ultraviolet detector of changeable wave length (Varian Model 2550) adjusted in 240 nm and a 4400 integratorSP Chromaject (Varian Associates, Inc., Sunnyvale, CA, USA). The extraction of the analyte resulted in recovery values between 90% and 108%, and variation coefficient enter 1,1% and 2.5%. The detention and quantification limits of the method were 0,02 and 0,04 μg mL-1, respectively. In conclusion, the analytical method possible the direct injection (on-line) of the sample without previous treatment also presenting some advantages, such as: fast, exactness, precision and specific.

scholarly journals RAPID ANALYTICAL METHOD FOR ASSAY DETERMINATION FOR PROCHLORPERAZINE EDISYLATE DRUG SUBSTANCES BY ULTRA PERFORMANCE LIQUID CHROMATOGRAPHY

2017 ◽  
Vol 9 (4) ◽  
pp. 118 ◽  
Author(s):  
Kishorkumar L. Mule
Keyword(s):  
Liquid Chromatography ◽  
Trifluoroacetic Acid ◽  
Analytical Method ◽  
Mobile Phase ◽  
Ultra Performance Liquid Chromatography ◽  
Drug Substance ◽  
Assay Method ◽  
Column Temperature ◽  
Drug Substances

Objective: To develop and validate new, simple and rapid assay method for Prochlorperazine edisylate drug substance by UPLC as per ICH guidelines.Methods: Ultra performance liquid chromatographic method was developed, optimized and validated on Acquity UPLC by using Acquity BDH300 C4 (100 x 2.1 mm) 1.7µ column. 3.85g ammonium acetate in 1000 ml of water add 0.5 ml trifluoroacetic acid and 1 ml triethylamine (Mobile phase A): 0.5 ml trifluoroacetic acid in 1000 ml acetonitrile mobile phase (Mobile phase B) with gradient program. Detector wavelength 254 nm and column temperature 30 °C.Results: Linearity study was carried out for prochlorperazine edisylate, linearity was calculated from 80 % level to 120% with respect to specification level. The correlation coefficient (r) = 0.999 was proved that the method is robust. The resolution between known impurities and Prochlorperazine edisylate found more than 2.5, it was evident from specificity test that Prochlorperazine edisylate peak are well separated from its related impurities, hence the method is specific. Prochlorperazine edisylate sample solution and mobile phase were found to be stable for at least 3 d.Conclusion: A new, simple and rapid method has been developed and validated for assay determination of prochlorperazine edisylate in drug substance by Ultra Performance Liquid Chromatography (UPLC). The analytical method was developed and validated as per ICH guidelines. The developed method can be used for the fast assay determination of prochlorperazine edisylate drug substances in research laboratories and in the pharmaceutical industry. 

scholarly journals New Method for the On-Line Determination of Molybdenum Via New Microphotometric Home Mode Instrument, Using Hight Emitting Diode as a Variable Intensity Radiant Source with a Miniture Photosilicone Diode Detector for System: Molybdenum(VI)-Hydrogen Peroxide-Ammonium Solution

2007 ◽  
Vol 4 (4) ◽  
pp. 571-582
Author(s):  
Baghdad Science Journal
Keyword(s):  
Hydrogen Peroxide ◽  
Classical Method ◽  
Wave Length ◽  
Research Work ◽  
Standard Addition ◽  
Ammonia Solution ◽  
Variable Intensity ◽  
Measurement Variation ◽  
On Line

This research work aims to the determination of molybdenum (VI) ion via the formation of peroxy molybdenum compounds which has red-brown colour with absorbance wave length at 455nm for the system of ammonia solution-hydrogen peroxide-molybdenum (VI) using a completely newly developed microphotometer based on the ON-Line measurement. Variation of responses expressed in millivolt. A correlation coefficient of 0.9925 for the range of 2.5-150 ?g.ml-1 with percentage linearity of 98.50%. A detection limit of 0.25 ?g.ml-1 was obtained. All physical and chemical variable were optimized interferences of cation and anion were studied classical method of measurement were done and compared well with newly on-line measurements. Application for the use of developed method on alloy samples, using standard addition method and agreed quite wall.

scholarly journals Therapeutic Drug Monitoring of Anticonvulsant Drugs by Micellar HPLC with Direct Injection of Serum Samples

2002 ◽  
Vol 48 (10) ◽  
pp. 1696-1702 ◽  
Author(s):  
Adrián Martinavarro-Domínguez ◽  
Maria-Elisa Capella-Peiró ◽  
Mayte Gil-Agustí ◽  
José V Marcos-Tomás ◽  
Josep Esteve-Romero
Keyword(s):  
Mobile Phase ◽  
Direct Injection ◽  
Sodium Dodecyl ◽  
Chromatographic Determination ◽  
Therapeutic Drug ◽  
Organic Modifiers ◽  
Serum Samples ◽  
Drug Concentrations ◽  
Mobile Phases

Abstract Background: We developed a micellar liquid chromatographic (MLC) procedure for the determination of three extensively monitored antiepileptics in serum samples: carbamazepine, phenobarbital, and phenytoin. Methods: We determined the composition of the mobile phase after modeling the elution behavior of the antiepileptics in hybrid micellar mobile phases of sodium dodecyl sulfate (SDS) with different organic modifiers (propanol, butanol, or pentanol) in an experimental design that used five mobile phases, a C18 column, and ultraviolet detection. In the micellar chromatographic system, the serum samples can be injected directly. Results: The optimum mobile phase was 70 mL/L butanol in 0.05 mol/L SDS, pH 7, in which the three antiepileptics were resolved in <10 min. Intra- and interday precision was evaluated at four different drug concentrations within the therapeutic range (n =10); CVs were <2.1%. The method was applied to the analysis of 120 serum samples, and results were similar to those obtained by the TDx® method. Conclusions: The MLC method allows chromatographic determination of three antiepileptics, using an interpretative strategy of optimization, without pretreatment of the serum samples and with direct injection in a hybrid micellar mobile phase of SDS–butanol. The method provides complete resolution and quantification of mixtures of two and three antiepileptics.

Determination of Chromium in Human Lung Fibroblast Cells Using a Large Bore—Direct Injection High-Efficiency Nebulizer with Inductively Coupled Plasma Mass Spectrometry

2000 ◽  
Vol 54 (5) ◽  
pp. 659-663 ◽  
Author(s):  
John A. McLean ◽  
Billy W. Acon ◽  
Akbar Montaser ◽  
Jatinder Singh ◽  
Daryl E. Pritchard ◽  
...  
Keyword(s):  
Inductively Coupled Plasma ◽  
High Efficiency ◽  
Human Lung ◽  
Direct Injection ◽  
Cell Mass ◽  
Lung Fibroblast ◽  
Fibroblast Cells ◽  
Human Lung Fibroblast ◽  
Inductively Coupled

A novel method for the determination of chromium in suspensions of human lung fibroblast cells is described by using a large bore–direct injection high efficiency nebulizer (LB-DIHEN) with micro-scale flow injection analysis and inductively coupled plasma mass spectrometric detection. Chromium(VI)-treated cells were first counted and then suspended in a phosphate buffer saline solution. With the use of the method of standard additions, the relative concentration of Cr in ∼ 100 HLF cells/peak was determined at m/z = 50. Because the cells tend to clump and can yield inhomogeneities in the total number analyzed, Mg was used as an internal standard to compensate for the total cell mass. The level of Cr in HLF cells grown in a medium of 100 μM Na2CrO4 for two hours is on the order of 180 fg Cr/cell after correction for the number of cells in each injection.

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