scholarly journals Use of High Performance Liquid Chromatography in the Analysis of a New Substance VMA-10-18

2021 ◽  
Vol 10 (3) ◽  
pp. 76-81
Author(s):  
E. S. Mischenko ◽  
J. S. Lazaryan ◽  
A. Jh. Lazaryan
Keyword(s):  
Ethyl Alcohol ◽  
Mobile Phase ◽  
High Performance ◽  
Orthophosphoric Acid ◽  
Statistical Processing ◽  
Biologically Active ◽  
Accuracy Class ◽  
Related Impurities ◽  
Relative Standard ◽  
Wide Range

Introduction. Quinazoline derivatives have a wide range of pharmacological properties, which makes this group quite unique among other classes of heterocyclic compounds. Substance VMA-10-18, which has cerebrovasodilating, antidepressant, anxiolytic and nootropic properties, may become a promising new drug. In this regard, an urgent task is to develop methods for standardizing this substance.Aim. Development of a method for the quantitation of related impurities of a new biologically active substance VMA-10-18 (Quinazophene) by HPLC with subsequent statistical processing of the results.Materials and methods. To develop the conditions for chromatographic analysis, was used a highly purified substance 3-[2-(4-methoxyphenylamino)-2-oxoethyl]-quinazolin-4(3H)-one, as well as its related impurities: impurity I (unsubstituted quinazolin-4(3H)-one) and impurity II (4-methoxychloroacetanilide). Test solutions were prepared using volumetric glassware of accuracy class 1. Ethyl alcohol 95 % was used as a solvent. Chromatography was performed using a Dionex UltiMate 3000 system (Dionex, United States) with a spectrophotometric detector. The analysis was carried out at a wavelength of 231 nm. Data collection and processing was carried out using the Chromeleon v.7 system. A mixture of acetonitrile and orthophosphoric acid was used as a mobile phase. The analysis was performed in an isocratic mode. The validation of the developed method was carried out taking into account the requirements of the State Pharmacopeia of Russian Federation XIV edition and the recommendations of the ICH.Results and discussion. The optimal conditions for chromatography of the VMA-10-18 substance and its impurities have been developed. It was found that for a clear separation of the peaks of the substance and impurities among themselves, the mobile phase should contain acetonitrile and orthophosphoric acid in a ratio of 80 : 20. The specificity of the method was determined by chromatography of ethyl alcohol in order to exclude its influence on the analysis results. The linearity and correctness of the method were determined at 7 levels of concentration of impurities of the substance. The correlation coefficient has exceeded 0.99. Also, the free term of the linear dependence equation (a) for both impurities was less than its confidence interval (Δа), which proves the absence of a systematic error of the method. When determining the "Convergence" indicator, the calculated relative standard deviation did not exceed 2 %. When determining the intralaboratory precision, Student's t-test and Fisher's F-test were calculated. Both indicators met the stated requirements.Conclusion. A method for the quantitative determination of impurities in the VMA-10-18 substance by HPLC has been developed and validated.

scholarly journals Development and Validation of Simple, Rapid and Sensitive High- Performance Liquid Chromatographic Method for the Determination of Butenafine Hydrochloride

2020 ◽  
pp. 116-125
Author(s):  
Mohammad Javed Ansari ◽  
Mohammed Muqtader Ahmed ◽  
Md. Khalid Anwer ◽  
Mohammed F. Aldawsari ◽  
Saad M. Al Shahrani ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Linear Regression Analysis ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Least Square ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Relative Standard ◽  
Wide Range

Aims: The current paper reports a simple, rapid, sensitive, accurate, and precise Reverse-phase high performance liquid chromatography (RP-HPLC) method with wide range of estimation to determine butenafine hydrochloride in nanosponges. This method has been validated as per ICH norms. Study Design:  Experimental design with influence of variables such as mobile phase composition, flow rate, temperature and wavelength on the chromatographic peaks. Place and Duration of Study: Department of Pharmaceutics, College of Pharmacy, Prince Sattam Bin Abdulaziz University, Al-Kharj, Saudi Arabia between Jan 2020 and March 2020. Methodology: Separation was achieved by utilizing the most commonly used reverse phase column (C-18, 5 μm, 150 mm x 4.6 mm) set at 30ºC and quantified by UV detection at 280 nm after isocratic elution from a mobile phase (70:30 v/v of methanol: phosphate buffer pH 3.0) flowing at 1 ml/min. Results: A sharp and symmetrical peak was observed at 4.08 ± 0.01 minutes. The low variation in peak area and retention time (1.12% and 0.29%, respectively) and a high number of theoretical plates (>2000) indicated this method’s efficiency and suitability. The least square linear regression analysis (Y = 9265.5 X + 1961.4) showed excellent correlation (r2 = 0.999 ± 0.0003) between concentration and peak area of butenafine hydrochloride through a wide concentration range of 1–50 µg/ml. The limits of detection and quantification (LOD and LOQ) were 0.18 µg/ml and 0.57 µg/ml, respectively. The assay or determinations were accurate, precise and reproducible with mean accuracy and mean relative standard deviation of precision of 101.53 ± 0.43% and 0.51 ± 0.11% respectively. Conclusion: The developed RP-HPLC method was simple, sensitive, reproducible with wide range of estimation of butenafine hydrochloride in the nanosponges. The proposed method could be used for the analysis of butenafine hydrochloride in the conventional pharmaceutical formulations such as tablets, syrup, creams including novel formulations such as nanoparticles, nanosponges, nanoemulsions. The proposed method overcomes the specificity, sensitivity and reproducibility related issues of ultraviolet-visible spectroscopy.

Phytochemical, Analytical and Medicinal Studies of Holoptelea integrifolia Roxb. Planch - A Review

2019 ◽  
Vol 5 (4) ◽  
pp. 270-277 ◽  
Author(s):  
Vijay Kumar ◽  
Simranjeet Singh ◽  
Ragini Bhadouria ◽  
Ravindra Singh ◽  
Om Prakash
Keyword(s):  
Liquid Chromatography ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
High Performance ◽  
Biologically Active ◽  
Toxicological Studies ◽  
Wide Range ◽  
Layer Chromatography

Holoptelea integrifolia Roxb. Planch (HI) has been used to treat various ailments including obesity, osteoarthritis, arthritis, inflammation, anemia, diabetes etc. To review the major phytochemicals and medicinal properties of HI, exhaustive bibliographic research was designed by means of various scientific search engines and databases. Only 12 phytochemicals have been reported including biologically active compounds like betulin, betulinic acid, epifriedlin, octacosanol, Friedlin, Holoptelin-A and Holoptelin-B. Analytical methods including the Thin Layer Chromatography (TLC), High-Performance Thin Layer Chromatography (HPTLC), High-Performance Liquid Chromatography (HPLC) and Liquid Chromatography With Mass Spectral (LC-MS) analysis have been used to analyze the HI. From medicinal potency point of view, these phytochemicals have a wide range of pharmacological activities such as antioxidant, antibacterial, anti-inflammatory, and anti-tumor. In the current review, it has been noticed that the mechanism of action of HI with biomolecules has not been fully explored. Pharmacology and toxicological studies are very few. This seems a huge literature gap to be fulfilled through the detailed in-vivo and in-vitro studies.

scholarly journals METHOD VALIDATION OF RIFAMPICIN ANALYSIS IN HUMAN PLASMA AND ITS APPLICATION IN BIOEQUIVALENCE STUDY

2019 ◽  
pp. 296-303
Author(s):  
ENDANG LUKITANINGSIH ◽  
FATHUL JANNAH ◽  
RATNA BUDHI PEBRIANA ◽  
RATNA DEWI PUSPITA ◽  
TAUFIQUROHMAN . ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Bioequivalence Study ◽  
Hplc Method ◽  
Coefficient Of Determination ◽  
European Medicines Agency ◽  
Pharmacokinetic Profiles ◽  
Relative Standard ◽  
Precision And Accuracy ◽  
Bioequivalence Test

Objective: This research aims to validate the method for rifampicin analysis in plasma by using High-Performance Liquid Chromatography (HPLC) that can be used to study the bioequivalence of a generic tablet of rifampicin 450 mg “X” marketed in Indonesia. Methods: Bioequivalence test was analysed using HPLC equipped with UV-Vis detector at 377 nm. The mobile phase used was acetonitrile-phosphate buffer pH 6.8 (45:55) delivered at a flow rate of 1.5 ml/min. Bioequivalence test was conducted on a limited number of subjects (n=8). The subjects were divided into two groups randomly. The pharmacokinetic profiles of the test tablet and reference tablet were statistically calculated using SPSS program to see the test tablet and reference tablet were bioequivalence or not. Results: The developed HPLC method for rifampicin analysis in plasma was sufficiently valid based on the International Conference on Harmonization (ICH) and European Medicines Agency (EMA) guideline, with precision and accuracy values were % Relative Standard Deviation (% RSD = 1.40–13.04) and % Recovery (86.24–102.13), respectively. Meanwhile, the method was linear over studied concentration (0.05 to 10.26 µg/ml) with a coefficient of determination (R2) = 0.9984. The method also had good stability and sensitivity. The result of statistical calculation showed that the generic rifampicin tablet X was bioequivalence toward the reference tablet Rimactan 450 mg. Conclusion: The test rifampicin tablet that was, the generic tablet “X” was bioequivalence toward the reference rifampicin tablet “Rimactan”.

scholarly journals Gradient HPLC in the determination of drug lipophilicity and acidity

2001 ◽  
Vol 73 (9) ◽  
pp. 1465-1475 ◽  
Author(s):  
Roman Kaliszan ◽  
Piotr Haber ◽  
Tomasz Baczek ◽  
Danuta Siluk
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Standard Procedure ◽  
Gradient Elution ◽  
Log P ◽  
Retention Data ◽  
Organic Modifier ◽  
Wide Range ◽  
Aqueous Component ◽  
Initial Ph

The linear-solvent strength (LSS) model of gradient elution in high-performance liquid chromatography (HPLC) has been demonstrated to provide parameters of lipophilicity and acidity of analytes. pKa and log kw values are determined in three gradient runs. The first two experiments use an aqueous buffered eluent with a wide-range organic modifier gradient at pH of buffer, providing suppression of ionization of the analyte. That experiment allows an estimate of contents of the organic modifier in the mobile phase (%B), producing requested retention coefficient, k, for the nonionized form of the analyte. The next experiment is carried out with the latter %B and a pH-gradient of the aqueous component of the eluent that is sufficient to overlap possible pKa value of the analyte. The initial pH of the buffer used to make the mobile phase is selected to insure that the analyte is in nonionized form. The resulting retention time allows an estimate of pKa in a solvent of the given %B.The log kw parameter obtained correlated well with the corresponding value obtained by the standard procedure of extrapolation of retention data determined in a series of isocratic measurements. The correlation between log kw and the reference parameter of lipophilicity, log P, was very good for a series of test analytes. The values of pKa were found to correlate with the literature pKa data determined in water for a set of aniline derivatives studied.

scholarly journals SENSITIVE DETERMINATION OF RELATED SUBSTANCES IN PIOGLITAZONE HYDROCHLORIDE BY HPLC

2017 ◽  
Vol 9 (2) ◽  
pp. 34
Author(s):  
N. Balaji ◽  
Sayeeda Sultana
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Internal Diameter ◽  
Related Substances ◽  
Relative Standard ◽  
Limit Of Quantitation

Objective: An efficient, high performance liquid chromatographic method has been developed and validated for the quantification of related substances in pioglitazone hydrochloride drug substance.Methods: This method includes the determination of three related substances in pioglitazone hydrochloride. The mobile phase A is 0.1% w/v triethylamine in water with pH 2.5 adjusted by dilute phosphoric acid. The mobile phase B is premixed and degassed mixtures of acetonitrile and methanol. The flow rate was 1 ml/min. The elution used was gradient mode. The HPLC column used for the analysis was symmetry C18 with a length of 250 mm, the internal diameter of 4.6 mm and particle size of 5.0 microns.Results: The developed method was found to be linear with the range of 0.006-250% with a coefficient of correlation 0.99. The precision study revealed that the percentage relative standard deviation was within the acceptable limit. The limit of detection and limit of quantitation of the impurities was less than 0.002%and 0.006% with respect to pioglitazone hydrochloride test concentration of 2000 µg/ml respectively. This method has been validated as per ICH guidelines Q2 (R1).Conclusion: A reliable, economical HPLC method was magnificently established for quantitative analysis of related substances of pioglitazone hydrochloride drug substance.

scholarly journals Development and validation of reversed phase high performance liquid chromatography (RP-HPLC) for quantification of captopril in rabbit plasma

2020 ◽  
Author(s):  
Muhammad Fawad Rasool ◽  
Umbreen Fatima Qureshi ◽  
Nazar Muhammad Ranjha ◽  
Imran Imran ◽  
Mouqadus Un Nisa ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Rabbit Plasma ◽  
Rp Hplc ◽  
Relative Standard

AbstractTh accurate rapid, simple and selective reversed phase high performance liquid chromatography (RP-HPLC) has been established and validated for the determination of captopril (CAP). Chromatographic separation was accomplished using prepacked ODSI C18 column (250 mm × 4.6 mm with 5 μm particle size) in isocratic mode, with mobile phase consisting of water: acetonitrile (60:40 v/v), pH adjusted to 2.5 by using 85% orthophosphoric acid at a flow rate of 1 mL/min and UV detection was performed at 203 nm. RP-HPLC method used for the analysis of CAP in mobile phase and rabbit plasma was established and validated as per ICH-guidelines. It was carried out on a well-defined chromatographic peak of CAP was established with a retention time of 4.9 min and tailing factor of 1.871. The liquid–liquid extraction method was used for extraction of CAP from the plasma. Excellent linearity (R2 = 0.999) was shown over range 3.125–100 µg/mL with mean percentage recoveries ranges from 97 to 100.6%. Parameters of precision and accuracy of the developed method meet the established criteria. Intra and inter-day precision (% relative standard deviation) study was also performed which was less than 2% which indicate good reproducibility of the method. The limit of detection (LOD) and quantification for the CAP in plasma were 3.10 and 9.13 ng/mL respectively. The method was suitably validated and successfully applied to the determination of CAP in rabbit plasma samples.

High Performance Liquid Chromatographic Determination of Primidone in Tablets

1982 ◽  
Vol 65 (5) ◽  
pp. 1063-1065
Author(s):  
Stanley E Roberts
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Average Recovery ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A high performance liquid chromatographic (HPLC) method is described for the quantitative determination of primidone in tablets. A ground tablet sample is diluted directly in the mobile phase, at a concentration of about 1 mg/mL of primidone, mixed and deaerated, and filtered. The resulting solution is then quantitated by HPLC. The average spike recoveries for the 50 mg and 250 mg tablets were 101.2% and 99.0%, respectively. The average recovery for an authentic mixture formulated at the 250 mg level was 100.1% with a relative standard deviation of 0.45%.

scholarly journals Application of Packed-nanofibers Solid-phase Extraction for Determination of Rhodamine B in Sausage

2019 ◽  
Vol 8 (1) ◽  
pp. 17-21
Author(s):  
Lanlan Wei ◽  
Jianjun Deng ◽  
Tao Kang ◽  
Xuejun Kang
Keyword(s):  
Rhodamine B ◽  
High Performance ◽  
Orthophosphoric Acid ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Volume Ratio ◽  
Standard Curve ◽  
Relative Standard ◽  
Limit Of Quantitation

A method for the determination of Rhodamine B in sausage was developed and validated. After extraction of Rhodamine B with acetonitrile from foodstuffs, a novel electrospun polymer nanofibers packed micro-column was used for cleaning and concentrating of the analyte in the sample. High performance liquid chromatography with fluorescence detection (HPLC-Flu) was used for the determination of Rhodamine B in the sample. The mobile phase was composed of 3.0 g L-1 phosphate buffer and methanol (3:7, volume ratio), and the pH was adjusted to 7. 0 with orthophosphoric acid. The results showed that the standard curve was linear over the validated concentrations range of 2-500 ng g-1, and the limit of detection (LOD) and the limit of quantitation (LOQ) for Rhodamine B spiked samples was 0. 2 ng g-1 and 0. 7 ng g-1, respectively. The average recoveries of Rhodamine B were 90.4% -94.3% for sausage, and the relative standard deviation of the method was from 1.7% to 3.8%. This proposed method was applied to real sample, and there was no Rhodamine B found in sausage.

scholarly journals Optimasi dan Validasi Metode Penentuan Kadar Asam Glikolat dan Asam Laktat Dalam Krim Menggunakan Kromatografi Cair Kinerja Tinggi

2020 ◽  
Vol 16 (1) ◽  
pp. 10
Author(s):  
Devi Wulandari ◽  
Gusrizal Gusrizal ◽  
Titin Anita Zaharah
Keyword(s):  
High Performance Liquid Chromatography ◽  
Lactic Acid ◽  
Liquid Chromatography ◽  
High Performance ◽  
Glycolic Acid ◽  
Orthophosphoric Acid ◽  
Spiked Sample ◽  
Relative Standard ◽  
Uv Visible

<p>Telah dilakukan optimasi dan validasi metode penentuan asam glikolat dan asam laktat dalam krim menggunakan kromatografi cair kinerja tinggi. Pemisahan asam glikolat dan asam laktat dilakukan pada kolom fasa balik C-8menggunakan fasa gerak asam ortofosfat 0,1% dengan pH 3,5 dan detektor <em>UV-Visible</em>. Standar asam glikolat dan asam laktat dibuat dengan melarutkannya menggunakan asam ortofosfat 0,1% pH 3,5. Hasil eksperimen menunjukkan bahwa pada rentang konsentrasi 25 – 400 μg/mL, asam glikolat dan asam laktat memiliki kurva yang linear dengan koefisien korelasi masing-masing 0,9997 dan 0,9999. Uji presisi untuk larutan standar berkonsentrasi 100 µg/mL menghasilkan simpangan baku relatif sebesar 1,49% untuk asam glikolat dan 1,72% untuk asam laktat. Metode yang telah dioptimasi memberikan akurasi yang baik yang ditunjukkan oleh nilai perolehan kembali dari pengukuran tiga <em>spiked sample</em> dengan konsentrasi berbeda (50, 100, dan 150 μg/mL). Nilai perolehan kembali untuk masing-masing konsentrasi <em>spiked sample</em> adalah 97,12% ± 0,69; 98,76% ± 0,43; 100,80% ± 0,29 untuk asam glikolat dan 97,58% ± 0,39; 96,20% ± 0,68; 98,00% ± 0,38 untuk asam laktat. Batas deteksi dan batas kuantisasi untuk asam glikolat adalah 0,05 dan 0,17 μg/mL, sedangkan untuk asam laktat adalah 1,40 dan 4,67 μg/mL. Nilai kekasaran metode untuk asam glikolat pada hari pertama dan hari kedua adalah 1,43% dan 1,67%, sedangkan untuk asam laktat adalah 1,67% dan 1,25%. Metode yang telah dioptimasi dan divalidasi berpotensi untuk digunakan secara spesifik pada penentuan kadar asam glikolat dan asam laktat dalam krim.</p><p><strong>Optimization and Validation of Determination Methods of Glycolic Acid and Lactic Acid in Cream Using High-Performance Liquid Chromatography.</strong> A high-performance liquid chromatography analytical method for the determination of glycolic acid and lactic acid in creams has been optimized and validated. The separation was performed in a reverse phase C–8 column with a mobile phase of 0.1%, orthophosphoric acid at pH 3.5, and UV-Visible detector. The standard of glycolic acid and lactic acid was dissolved in 0.1% orthophosphoric acid at pH 3.5. The experimental results showed that in the concentration range of 25–400 μg/mL, glycolic acid and lactic acid showed a linear curve with a correlation coefficient of 0.9997 and 0.9999, respectively. The precision test for standard solutions containing 100 µg/mL resulted in a relative standard deviation of 1.49% for glycolic acid and 1.72% for lactic acid. The optimized method provided good accuracy indicated by the recovery of the measurement of three spiked samples in different concentrations (50, 100, and 150 μg/mL). The recovery for each concentration of the spiked sample was 97.12% ± 0.69; 98.76% ± 0.43; 100.80% ± 0.29 for glycolic acid and 97.58% ± 0.39; 96.20% ± 0.68; 98.00% ± 0.38 for lactic acid. The limit of detection and limit of quantization for glycolic acid was 0.05 and 0.17 μg/mL, and for lactic acid was 1.40 and 4.67 μg/mL. The ruggedness of the method for glycolic acid on the first day and second day was 1.43% and 1.67%, while for lactic acid, it was 1.67% and 1.25%. The method that has been optimized and validated shows the potential to be used specifically for the determination of glycolic acid and lactic acid in the cream.</p>

scholarly journals RP-LC method for simultaneous determination of sulfamethoxazole and trimethoprim content in veterinary drugs

2015 ◽  
Vol 40 (1) ◽  
pp. 32 ◽  
Author(s):  
Gabriela Padovani Tahan ◽  
Simone Caetani Machado ◽  
Evandro Conti Malaguti ◽  
Patrícia Penido Maia ◽  
Susanne Rath ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Simultaneous Analysis ◽  
Ultraviolet Detector ◽  
Veterinary Medicines ◽  
Alternative Approach ◽  
Relative Standard ◽  
Water Ph ◽  
Comparison Of The Results

This study describes the development of a method for simultaneous analysis of sulfamethoxazole (SMX) and trimethoprim (TMP) through the use of high-performance liquid chromatography/ultraviolet detector, with the application to veterinary medicines. Satisfactory chromatographic separation of SMX and TMP was isocratically with a C18 column (150 x 4.6 mm, 5 mm). A mobile phase consisting of water, pH 3.5, and methanol (60:40, v/v) was delivered at a flow rate of 1.0 mL min-1 for five minutes and then, increased to 1.8 mL min-1. Detection of the drugs was performed at 213 and 230 nm. Linearity was demonstrated in the range of 5 to 70 mg mL-1 for SMX and 1 to 30 mg mL-1 for TMP (r2 ≥ 0.99 for both compounds). The relative standard deviation was ≤ 5%, and the comparison of the results with the concentrations reported on the drug labels indicated that the quantification was accurate. The resultant stressed samples were analysed by the method. The proposed method shows great potential for simultaneous analysis of the drugs evaluated and represents a new alternative approach to quality control of veterinary medicines.

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