scholarly journals Validated Method for the Determination of Piroxicam by Capillary Zone Electrophoresis and Its Application to Tablets

2014 ◽  
Vol 2014 ◽  
pp. 1-7 ◽  
Author(s):  
Arın Gül Dal ◽  
Zeynep Oktayer ◽  
Dilek Doğrukol-Ak
Keyword(s):  
Background Electrolyte ◽  
Internal Standard ◽  
Fused Silica ◽  
Electrophoretic Method ◽  
Pharmaceutical Tablets ◽  
Fused Silica Capillary ◽  
Capillary Zone ◽  
The Difference ◽  
Tablet Dosage

Simple and rapid capillary zone electrophoretic method was developed and validated in this study for the determination of piroxicam in tablets. The separation of piroxicam was conducted in a fused-silica capillary by using 10 mM borate buffer (pH 9.0) containing 10% (v/v) methanol as background electrolyte. The optimum conditions determined were 25 kV for separation voltage and 1 s for injection time. Analysis was carried out with UV detection at 204 nm. Naproxen sodium was used as an internal standard. The method was linear over the range of 0.23–28.79 µg/mL. The accuracy and precision were found to be satisfied within the acceptable limits (<2%). The LOD and LOQ were found to be 0.07 and 0.19 µg/mL, respectively. The method described here was applied to tablet dosage forms and the content of a tablet was found in the limits of USP-24 suggestions. To compare the results of capillary electrophoretic method, UV spectrophotometric method was developed and the difference between two methods was found to be insignificant. The capillary zone electrophoretic method developed in this study is rapid, simple, and suitable for routine analysis of piroxicam in pharmaceutical tablets.

Stability-Indicating Micellar Electrokinetic Chromatography Technique for Simultaneous Measurement of Delapril and Manidipine from a Combination Drug Formulation

2014 ◽  
Vol 97 (1) ◽  
pp. 114-120 ◽  
Author(s):  
Vítor Todeschini ◽  
Maximiliano da Silva Sangoi ◽  
Alianise da Silva Meira ◽  
Diogo Miron ◽  
Alini Dall Cortivo Lange ◽  
...  
Keyword(s):  
Background Electrolyte ◽  
Sodium Dodecylsulfate ◽  
Internal Standard ◽  
Fused Silica ◽  
Drug Formulation ◽  
Effective Length ◽  
Forced Degradation ◽  
Combination Drug ◽  
Stability Indicating ◽  
Fused Silica Capillary

Abstract A stability-indicating micellar electrokineticchromatography (MEKC) method was developed and validated for simultaneous analysis of delapril (DEL) and manidipine (MAN) using salicylic acid as an internal standard. The MEKC method was performed using a fused-silica capillary (effective length of 72 cm) with 50 mM of borate buffer and 5 mM of anionic surfactant sodium dodecylsulfate at pH9.0 as the background electrolyte. The separationwas achieved at 25 kV applied voltage and 35°C. The injection was performed at 50 mbar for5s, with detection at 208 nm. The method was linear in the range of 15–150 μg/mL (r2 = 0.9966) for DEL and 5–50 μg/mL (r2 = 0.9985) for MAN with adequate results for the precision (≤1.87%) and accuracy (98.94% for DEL and 100.65% for MAN). The specificity of the method and its stability-indicating capability was demonstrated through forced degradation studies, which showed that there was no interference from the excipients. The Plackett-Burman experimental design was used for robustness evaluation, giving results within the acceptable range. The method was successfully applied for analysis of the drugs, and the results were compared to an LC method, resulting in nonsignificant differences (P = 0.78 and0.84 for DEL and MAN, respectively).

scholarly journals Determination of Chlorinated Phenols in Water and Soil by Capillary Zone Electrophoresis

1997 ◽  
Vol 80 (6) ◽  
pp. 1308-1314 ◽  
Author(s):  
Wayne E Rae ◽  
Charles A Lucy
Keyword(s):  
Capillary Zone Electrophoresis ◽  
Fused Silica ◽  
Soil Samples ◽  
Chlorinated Phenols ◽  
Relative Standard ◽  
Zone Electrophoresis ◽  
Water And Soil Samples ◽  
Fused Silica Capillary ◽  
Capillary Zone

Abstract A capillary zone electrophoresis (CZE) method was developed to separate and determine chlorinated phenols in water and soil samples. A mixture of 16 chlorinated phenols was resolved in 25 min by using a 77 cm (70 cm to detector) × 75 μm fused silica capillary with 0.015M tetraborate/0.045M phosphate (pH 7.3) buffer at 22 kV. Calibration linearities for water samples in the low parts-permillion range were good (correlation coefficient &gt; 0.99) for all solutes except p-chlorophenol. Average precision was 17% relative standard deviation. Typical detection limits were in the 200 μg/L range. Recoveries of chlorinated phenols from synthetic soil samples with methanol were quantitative.

Determination of Ferulic Acid in “AI-FU-NUAN-GONG” Pills by High Performance Capillary Electrophoresis

2013 ◽  
Vol 850-851 ◽  
pp. 57-61
Author(s):  
Hai Xing Liu ◽  
Qing Liu ◽  
Xia Chen ◽  
Yan Fu Huan ◽  
Lin Tong Wang ◽  
...  
Keyword(s):  
Ferulic Acid ◽  
High Performance ◽  
Fused Silica ◽  
Borax Solution ◽  
Fused Silica Capillary ◽  
Capillary Zone ◽  
Good Repeatability ◽  
High Performance Capillary Electrophoresis ◽  
Silica Capillary Column

High performance capillary zone electrophoresis (HPCE) was used in this text to determine the content of ferulic acid in a ready-made Chinese herbal medicine called AI-FUNUAN-GONG (in pills). Electrophoretic separation conditions: Uncoated fused silica capillary column (75um×49/58cm), injection height 7.5cm, 30mmolL-1 borax solution, separation voltage 20kV, injection time 10s, detection wavelength 315 nm, experimental temperature 20°C.Linearity was kept in the concentration ranging from 1~62.5 mg·L-1 of ferulic acid with correlation coefficient of 0.970. The average recovery was 97.541% and RSD value was 6.57%. Sample content of ferulic acid was 0.0715mg/g. This method has the advantages of strong specificity, simpleness, speediness, accurate results and good repeatability in separation and it is useful for determination of ferulic Acid in AI-FU-NUAN-GONG Pills.

scholarly journals Validated Capillary Zone Electrophoretic Determination of Avanafil and Dapoxetine Hydrochloride in their Pure form and Pharmaceutical Preparation

2021 ◽  
pp. 446-459
Author(s):  
Mohamed B. Ali ◽  
Wael Talaat ◽  
Gamal A. Omran ◽  
Hassan A. M. Hendawy ◽  
Samir Morshedy
Keyword(s):  
Pharmaceutical Preparation ◽  
Background Electrolyte ◽  
Internal Standard ◽  
Fused Silica ◽  
Pure Form ◽  
Effective Length ◽  
Array Detector ◽  
Internal Diameter ◽  
Capillary Zone ◽  
Dapoxetine Hydrochloride

Aims: In this study, a simple, green, and rapid capillary zone electrophoresis (CZE) method coupled with a diode array detector (DAD) was applied for the analysis of avanafil (AVA) and dapoxetine hydrochloride (DAP) as a binary mixture using vardenafil (VAR) as an internal standard (IS) in pure form and pharmaceutical formulation. Methodology: The separation was done using fused silica capillary (58.5 cm total length, 50 cm effective length, and 50 μm internal diameter) and the running background electrolyte (BGE) was 100 mM acetate buffer at pH 3.6. During the separation process, the applied voltage was 30 KV, while the temperature was 25 °C. The sample injection was applied at a pressure of 50 mbar for 10 s, and detection was carried out at 210 nm for DAP and 248 nm for AVA and VAR. Results: Analysis of the tested drugs and the internal standard was carried out in less than 6.5 min, where the migration times were 4.29, 4.90, and 6.02 min for IS, DAP and AVA respectively. The proposed method showed linearity in the concentration range 5-80 and 5-70 μg/mL with correlation coefficients 0.9996 and 0.9999 for AVA and DAP respectively. The limit of detection (LOD) was 0.523 and 0.531 for AVA and DAP respectively, while the limit of quantification (LOQ) was 1.585 and 1.608 in respective order.  The Peak purity and identity in the proposed method were validated by DAD. Conclusion: The proposed CZE method was validated according to ICH guidelines and applied successfully for the estimation of AVA and DAP in their combined pharmaceutical preparation.

Capillary Zone Electrophoretic Determination of Histamine in Fish

1994 ◽  
Vol 77 (4) ◽  
pp. 881-884 ◽  
Author(s):  
Barry Mopper ◽  
Carl J Sciacchttano
Keyword(s):  
Food Poisoning ◽  
Fused Silica ◽  
Citrate Buffer ◽  
Coefficients Of Variation ◽  
Analytical Response ◽  
Fused Silica Capillary ◽  
Capillary Zone ◽  
Area Response ◽  
Silica Capillary

Abstract Histamine, the principal causative agent in scombroid food poisoning, was analyzed in seafood by a new, rapid, and sensitive method using capillary zone electrophoresis (CZE) with UV detection at 210 nm. Incurred histamine in methanolic fish extracts migrated within 4 min in a fused silica capillary filled with 0.02 M citrate buffer, pH 2.5, under an applied potential of 375 V/cm. The analytical response was linear from 0.5 to 100 ppm histamine (correlation coefficient, r = 0.999). The coefficients of variation for migration time and peak area response were &lt;1 and &lt;3%, respectively. Recovery of histamine in fortified fish composites was satisfactory. CZE was considered for alternative application in seafood speciation.

Evaluation of Enantioselective Capillary Electrophoretic Approach for the Enantiomeric Separation of Abscisic Acid

2020 ◽  
Vol 7 (1) ◽  
pp. 51-56
Author(s):  
Atiqah Binti Zaid ◽  
Udhayasurya N. Saravanan ◽  
Ng Woen Ching ◽  
Bahruddin Saad ◽  
Yong Foo Wong
Keyword(s):  
Abscisic Acid ◽  
Higher Plants ◽  
Background Electrolyte ◽  
Injection Pressure ◽  
Enantiomeric Separation ◽  
Fused Silica ◽  
Electrophoretic Method ◽  
Relative Standard ◽  
Fused Silica Capillary ◽  
Capillary Electrophoretic

Background: The application of enantioselective capillary electrophoresis approach for the assessment of the enantiomeric purity of chiral molecules is receiving increased attention. Abscisic acid is one of the chiral sesquiterpenic plant growth regulators that regulate various ecological and physiological roles in higher plants. Enantiomeric determination of ABA is of great concern because of the different biological activity of its enantiomers. Materials and Methods: In this study, we investigated the enantioseparation selectivity of ABA by incorporating native β-cyclodextrins (β-CD) and its derivatives as chiral modifiers in the background electrolyte of an enantioselective capillary zone electrophoresis system. Electrophoretic aspects that affect the enantiomeric separation, such as pH, types of β-CD and its concentration, applied voltage, injection pressure and time, were studied and optimised. Results and Discussions: An enhancement in enantioseparation was achieved in a bare fused-silica capillary (64.5 cm × 50 mm i.d.) using a background electrolyte solution consisting of (2-hydroxypropyl)- β-CD (80 mM) solubilised in 100 mM phosphate buffer adjusted to pH 5.9 with NaOH, operated under normal polarity mode (25 kV) at 25°C, and using hydrodynamic injection (75 mbar for 10s). Relative standard deviations of (intra- and inter-day) ≤ 3.23% and ≤ 1.39% for migration times and enantiomeric fractions (EF) were achieved using the proposed method. Conclusion: The proposed chiral capillary electrophoretic method offers advantages in terms of enantioselectivity and analysis times, which can serve as a reliable platform for the stereoisomeric analysis of ABA.

scholarly journals Determination of N-methyl-2-pyrrolidone and its metabolites in urine by micellar electrokinetic chromatography

2011 ◽  
Vol 9 (5) ◽  
pp. 825-833 ◽  
Author(s):  
Jana Lokajová ◽  
Simo Porras ◽  
Eivor Elovaara ◽  
Susanne Wiedmer
Keyword(s):  
Solid Phase ◽  
Background Electrolyte ◽  
Sodium Dodecyl ◽  
Fused Silica ◽  
Rat Urine ◽  
Fused Silica Capillary ◽  
On Line ◽  
Electrokinetic Capillary Chromatography ◽  
Silica Capillary

AbstractA fast and accurate micellar electrokinetic capillary chromatography (MEKC) method was developed for monitoring N-methyl-2-pyrrolidone (NMP) exposure. Baseline separation of NMP and its main metabolites: 5-hydroxy-N-methyl-2-pyrrolidone (5HNMP), N-methylsuccinimide (MSI), 2-hydroxy-N-methylsuccinimide (2HMSI), and 2-pyrrolidone (2P) was obtained within 6 min in an uncoated fused silica capillary using 5 mM phosphate buffer and 140 mM sodium dodecyl sulfate (pH 7.1) as background electrolyte (BGE). On-line UV-detection was performed at 200 nm and the applied electric field was 400 V cm−1. Possible interference of BGE-induced system peaks on separation was investigated by computer simulation and no such interference was observed. The developed MEKC method combined with solid phase extraction for sample preparation was successfully applied to the analysis of urine of rats exposed to NMP. The urinary excretion was determined in 0–6 h and 6–24 h specimens collected after an intragastic administration of 308 mg NMP / kg rat body weight. The results of NMP disposition kinetics in rat urine are reported for NMP and metabolites.

Validated Stability-Indicating Capillary Electrophoresis Method for the Separation and Determination of a Fixed-Dose Combination of Carvedilol and Hydrochlorothiazide in Tablets

2013 ◽  
Vol 96 (5) ◽  
pp. 951-959 ◽  
Author(s):  
Nourah Z Alzoman ◽  
Maha A Sultan ◽  
Hadir M Maher ◽  
Mona M AlShehri ◽  
Ileana V Olah
Keyword(s):  
Capillary Electrophoresis ◽  
Degradation Products ◽  
Background Electrolyte ◽  
Internal Standard ◽  
Fused Silica ◽  
Fixed Dose ◽  
Array Detector ◽  
Forced Degradation ◽  
Stability Indicating

Abstract A novel, fast, sensitive, and specific capillary electrophoresis (CE) technique coupled to a diode array detector has been developed for the separation and simultaneous determination of carvedilol (CRV) and hydrochlorothiazide (HCT) in two combination formulations. The proposed method utilized a fused silica capillary (55 cm × 75 μm id) and the background electrolyte solution phosphate buffer (12.5 mM, pH 7.4)–methanol (95 + 5, v/v). The separation was achieved at 30 kV applied voltage and 24°C. Atorvastatin (80 μg/mL) was chosen as the internal standard. The described method was linear over the range of 1–200 and 0.2–150 μg/mL for CRV and HCT, respectively. Intraday and interday RSD (n = 6) was ≤1.4%. The LOD values of CRV and HCT were 0.26 and 0.07 μg/mL, respectively. The validated CE method was successfully applied to the analysis of two commercial tablet dosage forms. Forced degradation studies were performed on bulk samples of the two drugs using thermal, photolytic, hydrolytic, and oxidative stress conditions, and the stressed samples were analyzed by the proposed method. Degradation products produced as a result of stress studies did not interfere with the determination of CRV and HCT; the assay could, therefore, be considered stability-indicating.

scholarly journals Validated capillary zone electrophoretic method for simultaneous analysis of benazepril in combination with amlodipine besylate and hydrochlorothiazide

2020 ◽  
Vol 32 (4) ◽  
pp. 219-227 ◽  
Author(s):  
Hytham M. Ahmed ◽  
Tarek S. Belal ◽  
Rasha A. Shaalan ◽  
Fawzy A. El Yazbi ◽  
Sohila M. Elonsy
Keyword(s):  
Antihypertensive Drugs ◽  
Limit Of Detection ◽  
Background Electrolyte ◽  
Fused Silica ◽  
Simultaneous Analysis ◽  
Effective Length ◽  
Array Detector ◽  
Amlodipine Besylate ◽  
Electrophoretic Method ◽  
Capillary Zone

In this work, a novel, simple, and quick capillary zone electrophoresis (CZE) method was proposed for simultaneous analysis of benazepril (BEN) with other co-administrated antihypertensive drugs, amlodipine besylate (AML) and hydrochlorothiazide (HCT), using a diode array detector (DAD). A fused silica capillary (78.5 cm total length, 70 cm effective length, and 75 μm id) was used in separation using a 40 mM phosphate buffer pH 7.5 as a running background electrolyte (BGE) under a positive potential of 30 KV, at a stable temperature of 25 °C for capillary during separation. Hydrodynamic injections were performed for 12 s at 50 mbar, and detection was performed at 210 nm for AML and BEN, at 225 nm for HCT, and at 232 nm for xipamide (XIP) added as an internal standard (IS). Separation of the three analyzed drugs and the IS was performed in less than 8 min. Migration times were 4.06, 5.23, 6.69, and 7.3 min for AML, HCT, BEN, and XIP, respectively. The findings proved that the proposed method was linear in the range of 10–80 μg/mL for all drugs with correlation coefficients >0.9994. The limit of detection (LOD) values of AML, HCT, and BEN were 1.004, 1.224, and 0.896 μg/mL, respectively, whereas the limit of quantification (LOQ) values were 3.124, 3.727, and 2.749 μg/mL for the cited drugs, respectively. Peak identity and purity were confirmed by DAD. The developed CZE method was applied for the analysis of the three antihypertensive drugs successfully in their combined pharmaceutical tablets, and it can be used for the quality control of single-pill combination (SPC) samples of these drugs in short time.

Determination of Musk Ambrette in Fragrance Products by Capillary Gas Chromatography with Electron Capture Detection: Interlaboratory Study

1994 ◽  
Vol 77 (6) ◽  
pp. 1467-1471 ◽  
Author(s):  
Harris H Wisneski ◽  
Ronald L Yates ◽  
Donald C Havery
Keyword(s):  
Electron Capture ◽  
Internal Standard ◽  
Fused Silica ◽  
Electron Capture Detection ◽  
Similar Response ◽  
Relative Standard ◽  
Fused Silica Capillary ◽  
Gas Chromatographic Method ◽  
Musk Ambrette

Abstract A gas chromatographic method that uses an internal standard additions technique is described for the determination of musk ambrette (MA) in fragrance products. A solution containing the product and a known amount of an internal standard, musk tibetene (MT), is injected directly into a gas chromatograph equipped with an electron capture detector. The chromatographic separation of the components on a wide-bore fused silica capillary column is recorded and a response constant is calculated from MA and MT peak heights. A similar response constant is also calculated for a standard solution containing known concentrations of MA and MT. The MA content of the fragrance product is then calculated. Average recoveries of MA from fragrance products ranged from 97.6 to 102.3%. The method was also evaluated collaboratively by 6 laboratories. In this study, the reproducibility relative standard deviation for MA in 6 fragrance test samples ranged from 2.78 to 22.87%.

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