scholarly journals A Rational Procedure to Increase Selectivity in the Determination of an Elicitor as Salicylic Acid in Polygala Extracts Using Capillary Electrophoresis

2021 ◽  
Author(s):  
Kheytiany Lopes ◽  
Tiago Tizziani ◽  
Ana Ruani ◽  
Luciano Vitali ◽  
Gustavo Micke
Keyword(s):  
Salicylic Acid ◽  
Background Electrolyte ◽  
Internal Standard ◽  
Isobutyric Acid ◽  
Migration Time ◽  
Rational Procedure ◽  
Capillary Zone ◽  
Standard Precision ◽  
Better Than

Considering the economic potential of secondary metabolites, researches have been focusing several strategies in order to explore and enhance the accumulation of these metabolites in plant matrices in a broad context. One of those strategies is the development of suitable methodologies for the determination of some elicitors, such as salicylic acid (SA). Since literature presents only a few analytical methods for the quantification of SA in plants, this study developed, validated and evaluated these metabolite contents in Polygala species using capillary zone electrophoresis with ultraviolet-visible detection. The background electrolyte (BGE) consisted of 15 mmol L−1 of hydroxymethyl-aminomethane and 30 mmol L−1 of 2-hydroxy-isobutyric acid, pH = 3.9. The BGE was chosen using a rational procedure to increase selectivity and reduce migration time. The method presented rapid performance, migration time less than 0.76 min for salicylic and phthalic acid (internal standard), precision results for peak area were better than 2.9% (intra-day) and 2.8% (inter-day) and the responses for the analytes were linear (range of 1-5 mg L−1), with limits of detection and quantification of 0.2 and 0.6 mg L−1, respectively. The developed method was applied for 39 samples of plant extracts.

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.

Gas Chromatographic-Thermal Energy Analysis Method for Determination of Volatile N-Nitrosamines in Baby Bottle Rubber Nipples: Collaborative Study

1987 ◽  
Vol 70 (1) ◽  
pp. 64-68 ◽  
Author(s):  
J Ian Gray ◽  
Michael A Stachiw
Keyword(s):  
Thermal Energy ◽  
Energy Analysis ◽  
Collaborative Study ◽  
Internal Standard ◽  
Analytical Techniques ◽  
The United States ◽  
Baby Bottle ◽  
Relative Standard ◽  
Better Than

Abstract A collaborative study was conducted on the U.S. Food and Drug Administration (FDA) dichloromethane extraction method for determining volatile N-nitrosamines in baby bottle rubber nipples. Following dichloromethane extraction, A'-nitrosamines were determined by gas chromatography-thermal energy analysis. Six pairs of blind duplicate rubber nipple samples representing 6 lots were analyzed by 11 collaborating laboratories. All samples were portions taken from equilibrated composites of cut-up rubber nipples obtained from manufacturers in the United States. Recoveries of the internal standard (N-nitrosodipropylamine) at approximately 20 ppb ranged from 10 to 120%. Reproducibility relative standard deviations (RSDJ were between 35 and 45% for N-nitrosamine levels from 10 to 20 ppb. However, when data from laboratories with recoveries less than 75% were excluded (this is now specified in the method), RSD„ values were between 11 and 32% for N-nitrosamine levels from 6 to 26 ppb. Values were consistent with or better than those reported for other analytical techniques designed to quantitate trace contaminants at the low ppb level, e.g., afiatoxin in foods. The method has been adopted official first action for the quantitation of volatile N-nitrosamines in baby bottle rubber nipples.

Determination of Ibuprofen in Human Plasma and Urine by Gas Chromatography/Mass Spectrometry

2014 ◽  
Vol 97 (2) ◽  
pp. 415-420 ◽  
Author(s):  
Bilal Yilmaz ◽  
Ali Fuat Erdem
Keyword(s):  
Human Plasma ◽  
Internal Standard ◽  
Gas Chromatography Mass Spectrometry ◽  
Oral Tablet ◽  
Liquid Liquid Extraction ◽  
Human Plasma And Urine ◽  
The Mean ◽  
Interday Precision ◽  
Better Than

Abstract This paper describes a GC/MS method for the determination of ibuprofen in human plasma and urine. Ibuprofen and internal standard naproxen were extractedfrom plasma and urine by using a liquid–liquid extraction method. Derivatization was carried outusing N-methyl-N-(trimethylsilyl) trifluoroacetamide. Calibration curves were linear over the concentration range of 0.05–5.0 and 0.1–10.0 μg/mL for plasma and urine, respectively. Intraday and interday precision (RSD) values for ibuprofen in plasma and urine were less than 6.31%, and accuracy (relative error) was better than 12.00%. The mean recovery of ibuprofen was 89.53% for plasma and 93.73% for urine. TheLOD was 0.015 and 0.03 μg/mL and the LOQ was 0.05 and 0.1 μg/mL for plasma and urine, respectively. The method was successfully applied to blood samples from three healthy male volunteers who had been given an oral tablet of 600 mg ibuprofen.

scholarly journals Green, Cost-Effective Simultaneous Assay of Chloramphenicol, Methylparaben, and Propylparaben in Eye-Drops by Capillary Zone Electrophoresis

2021 ◽  
Vol 2021 ◽  
pp. 1-11
Author(s):  
Thi Thanh Vuong Tong ◽  
Thi Thoa Cao ◽  
Nguyen Ha Tran ◽  
Thi Kim Van Le ◽  
Dinh Chi Le
Keyword(s):  
Capillary Zone Electrophoresis ◽  
Background Electrolyte ◽  
Cost Effective ◽  
Complete Separation ◽  
Sodium Tetraborate ◽  
Eye Drops ◽  
Solution Ph ◽  
Zone Electrophoresis ◽  
Capillary Zone

A green, cost-effective, and simple capillary zone electrophoresis (CZE) method was developed and validated for simultaneous determination of chloramphenicol, methylparaben, and propylparaben in eye-drops. With sodium tetraborate as background electrolyte (BGE), the apparent mobilities of chloramphenicol, methylparaben, and propylparaben increased and analysis time reduced when pH of BGE increased from 8.5 to 10.0 and concentration of BGE decreased from 40 mM to 15 mM, but complete separation of chloramphenicol from other matrix components was achieved only with sodium tetraborate concentration at 30 mM or higher and at pH = 9.3 or lower. The most suitable electrophoretic conditions for the intended application were a 30 mM sodium tetraborate solution, pH 9.3 as BGE, working voltage set at 25 kV, and UV detection at 280 nm at the cathodic extremity of the capillary. The final method was validated and proved to be reliable for assay of chloramphenicol, methylparaben, and propylparaben in eye-drops.

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.

scholarly journals Simultaneous determination of amoxicillin and clavulanic acid in pharmaceutical preparations by capillary zone electrophoresis

2016 ◽  
Vol 52 (2) ◽  
pp. 281-286 ◽  
Author(s):  
Gabriel Hancu ◽  
Anamaria Neacşu ◽  
Lajos Attila Papp ◽  
Adriana Ciurba
Keyword(s):  
Clavulanic Acid ◽  
Simultaneous Determination ◽  
High Performance ◽  
Background Electrolyte ◽  
Pharmaceutical Preparations ◽  
System Temperature ◽  
Electrophoresis Method ◽  
Capillary Zone ◽  
Antibacterial Spectrum

ABSTRACT Clavulanic acid enhances the antibacterial spectrum of amoxicillin by rendering most β-lactamase producing isolates susceptible to the drug. A fast, simple and efficient capillary electrophoresis method was developed for the simultaneous determination of amoxicillin and clavulanic acid from complex mixtures. Using a 25 mM sodium tetraborate as background electrolyte at a pH of 9.30, + 25 kV applied voltage, 25 °C system temperature, UV determination at 230 nm; we succeeded in simultaneous separation of amoxicillin and clavulanic acid in approximately 2 minutes. The analytical performance of the method was evaluated in terms of reproducibility, precision, accuracy, and linearity. The optimized analytical method was applied for the determination of the two analytes from combined commercial pharmaceutical preparations. This CE method is fast, inexpensive, efficient, and environmentally friendly when compared with the more frequently used high performance liquid chromatography methods described in the literature.

Determination of Sucrose Diacetate Hexaisobutyrate in Soft Drinks by Gas-Liquid Chromatographic Analysis of Isobutyric and Acetic Acid Components as Decyl Esters

1973 ◽  
Vol 56 (5) ◽  
pp. 1264-1266
Author(s):  
Henry B S Conacher ◽  
Rajinder K Chadha ◽  
Jagannath R Iyengar
Keyword(s):  
Acetic Acid ◽  
Quantitative Estimation ◽  
Internal Standard ◽  
Isobutyric Acid ◽  
Soft Drinks ◽  
Sucrose Esters ◽  
Decyl Acetate ◽  
Liquid Chromatographic Analysis ◽  
Liquid Chromatographic

Abstract A procedure is presented for the quantitative estimation of sucrose diacetate hexaisobutyrate in soft drinks based on quantitative determination of the acetic and isobutyric acid components. The method involves an acidcatalyzed transesterification of the sucrose esters with sulfuric acid in decanol followed by GLC analysis of the resulting decyl acetate and isobutyrate, using hexanoic acid as internal standard. Recoveries of sucrose diacetate hexaisobutyrate from drinks fortified with this compound ranged between 92.8 and 97.8% in calculations based on acetic acid content and between 97.1 and 99.3% in those based on isobutyric acid. The analysis of several commercialjdrinks gave sucrose ester contents ranging from 11.5 to 14.2 mg/10 fluid oz.

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