scholarly journals Analytical Separation of Closantel Enantiomers by HPLC

Molecules ◽  
2021 ◽  
Vol 26 (23) ◽  
pp. 7288
Author(s):  
Basma Saleh ◽  
Tongyan Ding ◽  
Yuwei Wang ◽  
Xiantong Zheng ◽  
Rong Liu ◽  
...  
Keyword(s):  
Trifluoroacetic Acid ◽  
Mobile Phase ◽  
High Performance ◽  
Enantiomeric Separation ◽  
Biological Research ◽  
The Novel ◽  
Column Temperature ◽  
Racemic Form ◽  
Mobile Phase Modifiers ◽  
Antiparasitic Drug

Closantel is an antiparasitic drug marketed in a racemic form with one chiral center. It is meaningful to develop a method for separating and analyzing the closantel enantiomers. In this work, two enantiomeric separation methods of closantel were explored by normal-phase high-performance liquid chromatography. The influences of the chiral stationary phase (CSP) structure, the mobile phase composition, the nature and proportion of different mobile phase modifiers (alcohols and acids), and the column temperature on the enantiomeric separation of closantel were investigated in detail. The two enantiomers were successfully separated on the novel CSP of isopropyl derivatives of cyclofructan 6 and n-hexane-isopropanol-trifluoroacetic acid (97:3:0.1, v/v/v) as a mobile phase with a resolution (Rs) of about 2.48. The enantiomers were also well separated on the CSP of tris-carbamates of amylose with a higher Rs (about 3.79) when a mixture of n-hexane-isopropanol-trifluoroacetic acid (55:45:0.1, v/v/v) was used as mobile phase. Thus, the proposed separation methods can facilitate molecular pharmacological and biological research on closantel and its enantiomers.

scholarly journals Direct Enantiomeric Separation and Determination of Hexythiazox Enantiomers in Environment and Vegetable by Reverse-Phase High-Performance Liquid Chromatography

2020 ◽  
Vol 17 (10) ◽  
pp. 3453
Author(s):  
Ping Zhang ◽  
Sheng Wang ◽  
Dongmei Shi ◽  
Yangyang Xu ◽  
Furong Yang ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Enantiomeric Separation ◽  
Reverse Phase ◽  
Column Temperature ◽  
Resolution Factor ◽  
Phase Temperature ◽  
Lower Temperature

In the present study, the direct enantiomeric separation of hexythiazox enantiomers on Lux cellulose-1, Lux cellulose-2, Lux cellulose-3, Lux cellulose-4, Lux amylose-1 and Chirapak IC chiral columns were carefully investigated by reverse-phase high-performance liquid chromatography (RP-HPLC). Acetonitrile/water and methanol/water were used as mobile phase at a flow rate of 0.8 mL·min−1. The effects of chiral stationary phase, temperature, thermodynamic parameters, mobile phase component and mobile phase ratio on hexythiazox enantiomers separation were fully evaluated. Hexythiazox enantiomers received a baseline separation on the Lux cellulose-3 column with a maximum resolution of Rs = 2.09 (methanol/water) and Rs = 2.74 (acetonitrile/water), respectively. Partial separations were achieved on other five chiral columns. Furthermore, Lux amylose-1 and Chirapak IC had no separation ability for hexythiazox enantiomers when methanol/water was used as mobile phase. Temperature study indicated that the capacity factor (k) and resolution factor (Rs) decreased with column temperature increasing from 10 °C to 40 °C. The enthalpy (ΔH) and entropy (ΔS) involved in hexythiazox separation were also calculated and demonstrated the lower temperature contributed to better separation resolution. Moreover, the residue analytical method for hexythiazox enantiomers in the environment (soil and water) and vegetable (cucumber, cabbage and tomato) were also established with reliable accuracy and precision under reverse-phase HPLC condition. Such results provided a baseline separation method for hexythiazox enantiomers under reverse-phase conditions and contributed to an environmental and health risk assessment of hexythiazox at enantiomer level.

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. 

Detection, Quantitation, and Identification of Residual Aminopenicillins by High-Performance Liquid Chromatography after Fluorescamine Derivation

2000 ◽  
Vol 63 (10) ◽  
pp. 1421-1425 ◽  
Author(s):  
CHIH-CHUN HONG ◽  
FUSAO KONDO
Keyword(s):  
Bovine Serum ◽  
Mobile Phase ◽  
High Performance ◽  
Serum Proteins ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Excitation Wavelength ◽  
Column Temperature ◽  
Solid Phase Extraction Cartridge ◽  
Mobile Phases

A high-performance liquid chromatographic (HPLC) method with fluorescence detection after precolumn fluorescamine derivation was developed to detect residues of two aminopenicillins, amoxicillin (AMPC) and ampicillin (ABPC), in bovine serum. Proteins in serum samples spiked with each of these penicillins were precipitated with sodium tungstate and sulfuric acid, centrifuged, and removed by passage through a C18 solid-phase extraction cartridge. After precolumn treatment of the extraction products of AMPC and ABPC with fluorescamine solution, HPLC analysis with fluorescence spectrophotometric detection at an excitation wavelength of 390 nm and an emission wavelength of 485 nm was performed to identify these products. Two mobile phases were used for residual analysis by the isocratic HPLC system. An ODP column (polyvinyl alcohol bonded with an octadecyl functional group) that can be used with strongly alkaline mobile phases (pH 2.0 to 13) was selected, and the column temperature was set at 40°C. A mobile phase comprising 100-mM K2HPO4 solution and acetonitrile (72:28, vol/vol), which yielded AMPC and ABPC retention times of 4.1 and 7.9 min, respectively, was suitable for detection of residual ABPC but not for residual AMPC because interference was caused by peaks of other extracted substances. When a mobile phase comprising a different ratio of 100-mM K2HPO4 solution and acetonitrile (78:22, vol/vol) was used, the retention times of AMPC and ABPC were 7.3 and 26.3 min, respectively, and both penicillins could be analyzed using this system. The calculated standard curves of the reaction products with both mobile phases were linear, and the correlation coefficients were greater than 0.999. The lower limit of detection was 10 ng/ml for both penicillins. Analysis of extracts from bovine serum spiked with AMPC and ABPC at a concentration of 1 μg/ml yielded recovery rates of 102.2 ± 5.5% and 79.0 ± 5.2%, respectively. This detection method may be useful for routine laboratory testing of AMPC and ABPC.

scholarly journals Study on chemical constituents of different species of Dendrobium

2020 ◽  
Vol 165 ◽  
pp. 05026
Author(s):  
Zhenghui Wan ◽  
Qingjun Huang
Keyword(s):  
Mobile Phase ◽  
Research Method ◽  
High Performance ◽  
Chemical Constituents ◽  
Chromatographic Peak ◽  
Column Temperature ◽  
Injection Volume ◽  
Chinese Pharmacopoeia ◽  
Processing Techniques ◽  
Theoretical Plates

The objective of this study is to determine the erianin of 10 species of Dendrobium by high performance liquid chromatography (HPLC). Processing techniques were washed, dried and ground. The research method for determining the content of erianin was adopted from Chinese Pharmacopoeia 2015 Edition. Acetonitrile-0.05% phosphoric acid (37:63) was used as mobile phase. The samples were separated on Sharpsil-TC18 column(4.6*150mm;5μm) at a flow rate of 1.2mL/min and detected at 230nm, and the column temperature was kept at 30℃. The injection volume was 20μL. The number of theoretical plates was not less than 6000 according to the chromatographic peak of erianin. The result of the study showed erianin was detected only in Dendrobium chrysotoxum among the 10 species of Dendrobium. and the content was 0.098%. Conclusion: The content of erianin in Dendrobium chrysotoxum met the specification of no less than 0.03% in the 2015 edition of Chinese Pharmacopoeia.

scholarly journals Chromatographic and Computational Studies on the Chiral Recognition of Sulfated β-Cyclodextrin on Enantiomeric Separation of Milnacipran

2020 ◽  
Author(s):  
Pranav Pathak ◽  
Evans C. Coutinho ◽  
Krishnapriya Mohanraj ◽  
Elvis Martis ◽  
Vikalp Jain
Keyword(s):  
Molecular Docking ◽  
Mobile Phase ◽  
Chiral Recognition ◽  
Cost Effective ◽  
Enantiomeric Separation ◽  
Enantiomeric Resolution ◽  
Recognition Mechanism ◽  
Column Temperature ◽  
Successful Resolution ◽  
Experimental Findings

<p></p><p>A new, cost-effective and fast chromatographic method using sulfated β-cyclodextrin (SβCD) as a chiral mobile phase additive (CMPA) was developed and validated for the enantiomeric separation of milnacipran. Milnacipran is an anti-depressant drug. Levo-milnacipran is the active enantiomer with less adverse effects than dextro-milnacipran. Hence, it is imperative to separate the enantiomers of milnacipran. Various parameters affecting enantiomeric resolution, for instance, the effect of type and concentration of cyclodextrins, the effect of pH of the mobile phase, effect of type and concentration of the organic solvent in the mobile phase and effect of type of achiral column, were investigated. We demonstrated successful resolution of enantiomers of milnacipran on reverse-phase HPLC with Kinetex C8 column (150x4.6mm, 5µ), using a mobile phase consisting of 18:82 v/v acetonitrile: 10mM sodium dihydrogen orthophosphate dihydrate buffer pH 3.0 (adjusted with orthophosphoric acid) containing 10mM SβCD with a flow rate 1.0 ml/minute. The column temperature was ambient and UV detection was carried out at 227 nm with an injection volume of 20µl. This method for enantiomeric separation of milnacipran was validated in accordance with ICH guidelines and successfully applied to the marketed formulation of Levomilnacipran. Furthermore, molecular docking was used to identify the chiral recognition mechanism. The results of molecular docking corroborated with our experimental findings.</p><br><p></p>

scholarly journals THE OPTIMIZATION OF HPLC FOR QUANTITATIVE ANALYSIS OF ACID ORANGE 7 AND SUDAN II IN COSMETIC PRODUCTS USING BOX BEHNKEN DESIGN

2019 ◽  
pp. 130-137 ◽  
Author(s):  
NOVALINA BR PURBA ◽  
ABDUL ROHMAN ◽  
SUDIBYO MARTONO
Keyword(s):  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
High Performance ◽  
Hplc Method ◽  
Acid Orange 7 ◽  
Column Temperature ◽  
Box Behnken Design ◽  
Acid Orange

Objective: The objective of this study was to optimize high-performance liquid chromatography (HPLC) method for the determination of acid orange 7 (AO7) and sudan II (SII) in blusher product based on response surface methodology using box behnken design (BBD) approach. Methods: Some factors responsible for HPLC separation including column temperature, mobile phase composition, flow rate were optimized using BBD. The responses evaluated were peak area, retention time, and tailing factor. AO7 and SII in blusher product has different properties, therefore both analytes were analysed using C18 column (Thermo Synergy Gold 250 mm x 4.6 mm i.d.,5 µm) using Shimadzu LC 20AD chromatograph equipped with photo-diode array (PDA) detector at 300-650 nm. The mobile phase used was acetonitrile-water (1:1 v/v), and acetonitrile composition was optimized at 35-50% for separation AO7 (ACN1), and 80-90% for SII (ACN2), delivered at the flow rate of 0.9–1 ml/min, using column temperature at 30-40 °C. Results: BBD showed that separation of AO7 was influenced by the concentration of ACN1, flow rate and column temperature. These factors affected retention time, peak area, and tailing factor with peak area was the most significant. Tailing factor was not significantly affected by each factor, and retention time was slightly effected. Otherwise, Sudan II was affected by all these factors except ACN1. The optimal condition obtained based BBD was ACN1 43%, ACN2 90%, the flow rate of 0.9 ml/min and a column temperature of 40 °C. Conclusion: BBD can be used to get optimum condition for analysis of AO7 and SII in blusher product.

Analysis of Bifenthrin and its Enantiomer Using High Performance Liquid Chromatography

2014 ◽  
Vol 675-677 ◽  
pp. 275-279 ◽  
Author(s):  
Su Su Fan ◽  
Jian Shi ◽  
Ling Zhou ◽  
Yu Wen Hang
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Chiral Stationary Phase ◽  
Ammonium Acetate ◽  
Hplc Method ◽  
Column Temperature ◽  
Polysaccharide Derivatives ◽  
Separation Results

Using the high performance liquid chromatography (HPLC) method, bifenthrin isomers can be split at a polysaccharide derivatives chiral stationary phase column, and two well distinguished peaks of bifenthrin isomers are obtained. The effects of mobile phase ratios, temperatures, and detection wavelengths on the separation results are discussed. The optimal chromatographic conditions are as follows: the mobile phase ratio is methanol: ammonium acetate salts = 80:20, the column temperature is 35°C, and the wavelength is set as 220 nm. Under the optimal conditions, the resolution of bifenthrin enantiomer can be as large as 3.0.

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