scholarly journals Determination of Magnesium Valproate and Its Process Related Impurities by Ultraperformance Liquid Chromatography

2014 ◽  
Vol 2014 ◽  
pp. 1-6
Author(s):  
Rakshit Thakkar ◽  
Hitesh Saravaia ◽  
Madhavi Patel ◽  
Anamik Shah
Keyword(s):  
Mobile Phase ◽  
Reversed Phase ◽  
Isocratic Elution ◽  
Related Impurities ◽  
System Suitability ◽  
Liquid Chromatographic ◽  
Ammonium Dihydrogen Orthophosphate ◽  
Dihydrogen Orthophosphate

A selective ultraperformance liquid chromatographic (UPLC) method for the determination of magnesium valproate and its process related impurities has been developed. The method includes reversed-phase Acquity BEH C18 column with 100 mm × 2.1 mm i.d. and 1.7 µ particle size. The mobile phase consists of acetonitrile and 5 mM ammonium dihydrogen orthophosphate with pH = 3.0 at 45 : 55 isocratic elution. The flow rate was set at 0.3 mL/min and UV detection was performed at 215 nm. A system suitability test (SST) was developed to govern the quality of the separation. The developed method has been validated further with respect to linearity, accuracy, precision, selectivity, LOD, LOQ, and robustness. Different batches of samples were examined using this method; the method proved to be successful when applied to analyze a marketed magnesium valproate formulation.

scholarly journals An Isocratic Method for Quantification of Valproic Acid and Its Related Impurities Using Ion Pair Reagent by Ultraperformance Liquid Chromatography

2012 ◽  
Vol 2012 ◽  
pp. 1-5 ◽  
Author(s):  
Rakshit Thakkar ◽  
Hitesh Saravaia ◽  
Mrunal Ambasana ◽  
Madhavi Patel ◽  
Anamik Shah
Keyword(s):  
Valproic Acid ◽  
Mobile Phase ◽  
Reversed Phase ◽  
Ion Pair ◽  
Related Impurities ◽  
Acid Sodium Salt ◽  
System Suitability ◽  
Liquid Chromatographic ◽  
Salt Flow

A selective ultraperformance liquid chromatographic (UPLC) method for the quantification of valproic acid and its known related impurities using ion pair reagent has been developed. The method includes reversed-phase Acquity HSS T3 column with 100 mm × 2.1 mm i.d. and 1.7 μ particle size. The mobile phase consists of acetonitrile, 5 mM 1-hexanesulphonic acid sodium salt, flow rate is 0.6 mL/min, and UV detection is performed at 215 nm. A system suitability test (SST) was developed to govern the quality of the separation. The developed method has been validated further with respect to linearity, accuracy, precision, selectivity, LOD, LOQ, and Robustness.

Improved liquid-chromatographic determination of haloperidol in plasma.

1984 ◽  
Vol 30 (7) ◽  
pp. 1228-1230 ◽  
Author(s):  
A K Dhar ◽  
H Kutt
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Room Temperature ◽  
Internal Standard ◽  
Isoamyl Alcohol ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract This method for determination of haloperidol in plasma is based on "high-performance" isocratic liquid chromatography with the use of a C8 bonded reversed-phase column at room temperature. Haloperidol and the internal standard (chloro-substituted analog) are extracted from alkalinized plasma into isoamyl alcohol/heptane (1.5/98.5 by vol) and back-extracted into dilute H2SO4. The aqueous phase is directly injected onto the column. The mobile phase is a 30/45/25 (by vol) mixture of phosphate buffer (16.5 mmol/L, pH 7.0), acetonitrile, and methanol. Unlike other liquid-chromatographic procedures for haloperidol, commonly used psychotropic drugs do not interfere. Analysis can be completed within an hour. The procedure is extremely sensitive (1.0 microgram/L) and is well reproducible (CV 5.6% for a 2.5 micrograms/L concentration in plasma).

Determination of Cymiazole Residues in Honey by Liquid Chromatography

1993 ◽  
Vol 76 (1) ◽  
pp. 92-94 ◽  
Author(s):  
Paolo Cabras ◽  
Marinella Melis ◽  
Lorenzo Spanedda
Keyword(s):  
Liquid Chromatography ◽  
Chromatographic Analysis ◽  
Mobile Phase ◽  
Chromatographic Method ◽  
Reversed Phase ◽  
Limit Of Determination ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic ◽  
Control Samples

Abstract A liquid chromatographic method is described for the determination of cymiazole residues in honey. This acaricide is determined on a reversed-phase (C18) column, with a CH3CN-O.OOIN HCI-NaCI mixture (950 mL + 50 mL + 0.3 g/L) as the mobile phase, and UV detection at 265 nm. Cymiazole is extracted with n-hexane from aqueous alkalinized (pH 9) honey solutions. No further cleanup of the honey extract was required before chromatographic analysis. Recoveries on control samples fortified with 0.01,0.10, and 1.00 ppm cymiazole ranged from 92 to 102%. The limit of determination was 0.01 ppm.

scholarly journals Improved Liquid Chromatographic Method for Determination of Organic Acids in Leaves, Pulp, Fruits, and Rinds of Garcinia

2003 ◽  
Vol 86 (5) ◽  
pp. 1063-1068 ◽  
Author(s):  
Guddadarangavvanahally K Jayaprakasha ◽  
Bhabani S Jena ◽  
Kunnumpurath K Sakariah
Keyword(s):  
Organic Acids ◽  
Mobile Phase ◽  
Reversed Phase ◽  
Direct Application ◽  
Improved Method ◽  
Hydroxycitric Acid ◽  
Liquid Chromatographic Method ◽  
Acid Lactone ◽  
Liquid Chromatographic

Abstract An improved liquid chromatographic (LC) method was developed for determination of organic acids in leaves, pulp, fruits, and rinds of Garcinia. At present, the commonly used LC method for analysis of organic acids in Garcinia extracts uses direct application of the extracts on the column. This practice gradually reduces efficiency of the column and shortens its life. In the improved method, the interfering substances such as pigments and xanthones were effectively removed by passing the aqueous extract through an ODS cartridge. With subsequent injection on a C18 reversed-phase column, using 6.0mM phosphoric acid as the mobile phase with a flow rate of 1.0 mL/min and UV detection at 210 nm, the organic acids were determined in the extracts. The major organic acid was (–)-hydroxycitric acid at the level of 2.5, 0.8, 3.0, and 20.1% in leaf, pulp, fresh fruit, and dried rinds, respectively. Minor quantities of hydroxycitric acid lactone, oxalic acid, and citric acid were also identified. Limits of detection and recoveries were 0.9–1.5 μg and 93.9–99.8%, respectively. This is the first report on the composition of organic acids from Garcinia pedunculata.

Improved liquid-chromatographic determination of 3-methoxy-4-hydroxyphenylethyleneglycol in urine with electrochemical detection.

1984 ◽  
Vol 30 (1) ◽  
pp. 140-143 ◽  
Author(s):  
J R Shipe ◽  
J Savory ◽  
M R Wills
Keyword(s):  
Mobile Phase ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Improved Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Mean Concentration ◽  
Phase Column

Abstract In this improved method for quantifying 3-methoxy-4-hydroxyphenylethyleneglycol (MHPG) in urine, after a multistep extraction of MHPG and internal standard (iso-MHPG) from 3.0 mL of urine, the compounds are separated on a C18 reversed-phase column and quantified by use of an electro-chemical detector. The isocratic chromatographic separation takes about 16 min. The mobile phase is phosphate buffer/acetonitrile (88/12 by vol), the flow rate 0.7 mL/min. Recycling the mobile phase and automating the sample injection make possible the unattended assay of more than 70 samples per day. The within-run precision of the method is excellent (CV 1.8%) at a mean concentration of 1.1 mg/L.

Liquid Chromatographic Determination of Vitamin D in Animal Feeds and Premixes

1992 ◽  
Vol 75 (5) ◽  
pp. 812-814 ◽  
Author(s):  
Vipin K Agarwal
Keyword(s):  
Vitamin D ◽  
Mobile Phase ◽  
Potassium Hydroxide ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Ultraviolet Detection ◽  
Animal Feeds ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method has been developed for the determination of vitamin D (D2 + D3) in animal feeds and premixes. The sample is saponified with potassium hydroxide, and vitamin D is extracted with hexane and isomerized to isotachysterol with 10M HCI in 2-butanol. LC determination of isotachysterol to quantitate vitamin D is carried out on a reversed-phase column with acetonitrilemethanol (90 +10) as the mobile phase and ultraviolet detection at 301 nm. The detection limit of the method is 1 lU/g. This method can also be used for the determination of vitamin D2 and D3 separately.

scholarly journals DEVELOPMENT AND VALIDATION OF A HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD DETERMINATION OF ZIDOVUDINE ENCAPSULATED IN PCL NANOPARTICLES

2017 ◽  
Vol 1 (2) ◽  
pp. 1-8
Author(s):  
Milena Cristina Ribeiro Souza Magalhães ◽  
Alisson Samuel Portes Caldeira ◽  
Hanna De Sousa Rocha Almeida ◽  
Sílvia Ligório Fialho ◽  
Armando Da Silva Cunha Junior
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Liquid Chromatographic Method ◽  
Development And Validation ◽  
Liquid Chromatographic ◽  
Isocratic Mode

A reversed-phase high-performance liquid chromatographic (HPLC) method was developed and validated for the determination of encapsulation efficiency of zidovudine in nanoparticules. The method was carried out in isocratic mode using 0.040M sodium acetate: methanol: acetonitrile: glacial acetic acid (880:100:20:2) as mobile phase, a C8 column at 25ºC and UV detection at 240 nm. The method was linear (r2 ˃ 0.99) over the range of 25.0-150.0 μg/mL, precise (RSD ˂ 5%), accurate (recovery = 100.5%), robust and selective. The validated HPLC-UV method can be successfully applied to determine the rate of zidovudine in nanoparticules.

A high-performance liquid-chromatographic method for routine simultaneous determination of nicotine and cotinine in plasma.

1988 ◽  
Vol 34 (4) ◽  
pp. 724-729 ◽  
Author(s):  
M Hariharan ◽  
T VanNoord ◽  
J F Greden
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
High Performance ◽  
Methylene Chloride ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Standard Curve ◽  
Liquid Chromatographic

Abstract We describe a rapid, sensitive method for the routine simultaneous determination of nicotine and cotinine in 1 mL of plasma. Extraction in 10-mL screw-capped Teflon tubes with methylene chloride after deproteinization with trichloroacetic acid eliminated emulsion formation. The extract, after evaporation and reconstitution in 30 microL of mobile phase, is injected into a reversed-phase C-18 ion-pair column of an isocratic high-performance liquid-chromatographic unit. Absorbance is monitored at 256 nm. The mobile phase is a citrate-phosphate (30 mmol each per liter) buffer mixture containing 50 mL of acetonitrile and 1 mmol of sodium heptanesulfonate per liter. 2-Phenylimidazole is the internal standard. The detection limit is 1 microgram/L for nicotine and 3 micrograms/L for cotinine. The standard curve is linear from 0 to 700 micrograms/L for both compounds. The average CV for nicotine in the concentration range 0-100 micrograms/L is 6.5%, and that for cotinine in the concentration range 50-700 micrograms/L is 4%.

Liquid-chromatographic determination of pentobarbital in plasma with use of a resin column and an alkaline mobile phase.

1982 ◽  
Vol 28 (8) ◽  
pp. 1772-1774 ◽  
Author(s):  
R N Gupta ◽  
P T Smith ◽  
F Eng
Keyword(s):  
Mobile Phase ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Enhanced Sensitivity ◽  
Acidic Drugs ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract We describe a liquid-chromatographic method involving a new, nonsilica column (XAD-2, Hamilton Co.) for pentobarbital in plasma. Plasma is extracted with chloroform after addition of the internal standard, 5-ethyl-5-p-tolyl-barbituric acid. Acidic drugs are back-extracted into alkali, then chromatographed on the resin-base reversed-phase column. The use of alkaline mobile phase allows enhanced sensitivity and detection of barbiturates at 240 nm. The within-run CV for 10 samples was 1.9%, the between-run CV 1.8%. Ten commonly used barbiturates are separated isocratically in less than 15 min. Other commonly prescribed acidic drugs do not interfere with determination of pentobarbital.

scholarly journals Simultaneous Determination of E- and Z-Guggulsterones in Dietary Supplements Containing Commiphora mukul Extract (Guggulipid) by Liquid Chromatography

2001 ◽  
Vol 84 (1) ◽  
pp. 24-28 ◽  
Author(s):  
Mythili Nagarajan ◽  
Ted W Waszkuc ◽  
Jidong Sun
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Reversed Phase ◽  
Liquid Chromatographic Method ◽  
Commiphora Mukul ◽  
Hypolipidemic Agent ◽  
Synthetic Standard ◽  
Cis And Trans ◽  
Liquid Chromatographic

Abstract Guggulipid, the standardized product from the extraction of the ole-gum-resin from the Commiphora mukul plant, has been marketed as a hypolipidemic agent. The ketosteroids, cis- and trans-4,17(20)-pregnadiene-3,16-dione, known as E- and Z-guggulsterones, respectively, are the main ingredients in guggulipid. A liquid chromatographic method was developed for simultaneous determination of E- and Z-guggulsterones in guggulipid preparations using synthetic E- and Z-guggulsterone standards. Realtively low amounts of guggulsterones (E and Z) were found in commercial guggulipid preparations in comparison with the manufacturer's claim of 2.5%. The mixture of E- and Z-guggulsterones was extracted and separated on a Symmetry C18 reversed-phase column, with a mobile phase of acetonitrile–water (46 + 54, v/v) and detected at 242 nm. The retention times of E- and Z-guggulsterones are approximately 8 and 11 min, respectively. Assay quantitation was based on the calibration curve obtained from a mixture of synthetic standard E- and Z-guggulsterones. Experimental data on selectivity, linearity, accuracy, and recoveries are presented.

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