scholarly journals Simultaneous HPLC estimation of Amphetamine and Caffeine abuse drugs in Iraqi human addicts

2021 ◽  
Vol 4 (1) ◽  
pp. 25-31
Author(s):  
Rulla Sabah
Keyword(s):  
Particle Size ◽  
High Performance Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Linear Regression Analysis ◽  
Analysis Data ◽  
Hplc Separation ◽  
Isocratic Elution ◽  
Diethyl Amine ◽  
Buffer Value

The main aim of this research is to establish and validate a high performance liquid chromatography (HPLC) process for the separation and estimation of Amphetamine (AM) and Caffeine (CAF) in its illegal formula and in sera of addicts. This method is established on the HPLC separation of the two drugs on the ZORBAX ODS column (250×4.6×5µm particle size). The mobile phase contained 1% ortho-phosphoric acid 85% and 1%of diethyl amine 99%, acetonitrile and methanol ratio was 85:10:5 v/v/v. The flow rate is 1.2 mL.min-1, buffer value pH of 2.5 via isocratic elution also UV detection at 210 nm. The retention times for the two drugs AM and CAF were obtained at 4.425 and 6.456 min, respectively. The calibration curves founded that the linear regression analysis data gave a good linear relationship for the concentration range 1 to 100 µg.mL-1 for AM and CAF. The values achieved for correlation coefficient, slope and intercept were 9999, 8104.2 and 5012 for AM and 0.9999, 9698.5 and 6342.9 for CAF, whereas the LOD and LOQ was 0.51, 1.64 µg.mL-1 for AM and 0.60, 1.32 µg.mL-1 for CAF  

Analysis of organic impurities of besifloxacin hydrochloride by high performance liquid chromatography with isocratic and gradient elution.

2019 ◽  
Vol 16 ◽  
Author(s):  
Joanna Wittckind Manoel ◽  
Camila Ferrazza Alves Giordani ◽  
Livia Maronesi Bueno ◽  
Sarah Chagas Campanharo ◽  
Elfrides Eva Sherman Schapoval ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Gradient Elution ◽  
Pharmaceutical Product ◽  
Raw Material ◽  
Isocratic Elution ◽  
Organic Impurities ◽  
Elution Method

Introduction: Impurity analysis is an important step in the quality control of pharmaceutical ingredients and final product. Impurities can arise from drug synthesis or excipients and even at small concentrations may affect product efficacy and safety. In this work two methods using high performance liquid chromatography (HPLC) were developed and validated for the evaluation of besifloxacin and its impurity synthesis, with isocratic elution and another with gradient elution. Method: The analysis by HPLC in isocratic elution mode was performed using a cyano column maintained at 25 °C. The mobile phase was composed by 0.5% triethylamine (pH 3.0): acetonitrile (88:12 v/v) eluted at a flow rate of 1.0 ml/min with detection at 330 nm. The gradient elution method was carried out with the same column and mobile phase components only modifying the rate between organic and aqueous phase during analysis. The procedures have been validated according to internationally accepted guidelines, observing results within acceptable limits. Results: The methods presented were found to be linear in the 140 to 260 µg/ml range for besifloxacin and 0.3 to 2.3 µg/ml for an impurity named A. The limits of detection and quantification were respectively 0.07 and 0.3 µg/ml for impurity A, with a 20 µL injection volume. The precision achieved for all analyses performed provided RSD inter-day equal to 6.47 and 6.36% for impurity A with isocratic elution and gradient, respectively. The accuracy was higher than 99% and robustness exhibited satisfactory results. In the isocratic method an analysis time of 25 min and 15 min was obtained for gradient. For impurity A, the number of theoretical plates in the isocratic mode was about 5000 while in the gradient mode it was about 45000, hence, it made the column more efficient by changing the mobile phase composition during elution. In besifloxacin raw material and in pharmaceutical product used in this study, other related impurities were present but but impurity A was searched for and not detected Conclusion: The proposed methods can be applied for quantitative determination of impurities in the analysis of the besifloxacin raw material, as well as in ophthalmic suspension of the drug, considering the quantitation limit.

scholarly journals HPLC determination of hydrochlorothiazide in urine after solid-phase extraction

2005 ◽  
Vol 51 ◽  
pp. 23-28 ◽  
Author(s):  
Violeta Ivanova ◽  
Dragica Zendelovska ◽  
Marina Stefova
Keyword(s):  
Particle Size ◽  
Solid Phase Extraction ◽  
Mobile Phase ◽  
Solid Phase ◽  
Hplc Method ◽  
Phase Extraction ◽  
Hplc Separation ◽  
Isocratic Elution ◽  
Extraction Recovery

A simple, rapid and precise HPLC method has been developed for the assay of hydrochlorothiazide in urine. The clean-up of the urine samples was carried out by solid-phase extraction using HLB cartridges. Extraction recovery was 94.00-100.28 %. HPLC separation was performed with isocratic elution on Hypersil BDS C18 column (100 x 4.0 mm I.D., 3 µm particle size) protected with appropriate guard column. The mobile phase was 18 % acetonitrile and 0.025 mol/L solution of KH2PO4, pH 4 at flow rate of 0.3 mL/min. Detection of the substances was performed at 220 nm. The calibration curves were linear in the range of 2-50 µg/mL. The developed method is validated by checking its accuracy, precision and stability. The detection limit is 2 µg/mL hydrochlorothiazide. The method is proved to be convenient for routine analysis of hydrochlorothiazide in urine.

scholarly journals Simultaneous Determination of Phenolic Compounds in Leptadenia pyrotechnica (Forssk.) Decne. by Using High-Performance Liquid Chromatography (HPLC-DAD-UV)

2018 ◽  
Vol 2018 ◽  
pp. 1-4
Author(s):  
Raman Preet ◽  
Raghbir Chand Gupta
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Phenolic Compounds ◽  
Mobile Phase ◽  
High Performance ◽  
Isocratic Elution ◽  
Methanolic Extracts ◽  
Aerial Parts ◽  
Whole Plant

During the present study, an endeavor has been made to produce a simple, rapid, and simultaneous method for determination of phenolic compounds by using high-performance liquid chromatography in aerial parts of Leptadenia pyrotechnica (Forssk.) Decne. collected from the Indian Thar Desert. The optimized process was used for the quantification of ten phenolic compounds. The chromatographic separation was accomplished on an Atlantis T3 column at 25°C with isocratic elution. A mixture of acetonitrile and water was used as the mobile phase at a flow rate of 0.8 mL/min. The linear regression examination data for the calibration plots displayed a good linear relationship with r2 > 0.999 in the concentration range of 2–20 µL. In the methanolic extracts of the whole plant of L. pyrotechnica, the content of caffeic acid (3.3%) was reported to be the highest concentration.

scholarly journals Determination of the Analgesic Components of Spasmomigraine® Tablet by Liquid Chromatography with Ultraviolet Detection

2007 ◽  
Vol 90 (1) ◽  
pp. 94-101 ◽  
Author(s):  
Fawzy A Elbarbry ◽  
Mokhtar M Mabrouk ◽  
Mohamed A El-Dawy
Keyword(s):  
Particle Size ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Ambient Temperature ◽  
Mobile Phase ◽  
High Performance ◽  
Internal Standard ◽  
Dosage Forms ◽  
Ultraviolet Detection

Abstract A procedure was developed for the determination of the analgesic components of Spasmomigraine® tablets, which are ergotamine (I), propyphenazone (II), caffeine (III), camylofin (IV), and mecloxamine (V). They were subjected to high-performance liquid chromatography on a column (300 × 3.9 mm, 10 μm particle size) packed with μ-Bondapak C18. Separations were achieved with the mobile phase methanol–water–triethylamine (60 + 40 + 0.1, v/v/v) flowing at a rate of 1.5 mL/min, and quantitative determination was performed at 254 nm at ambient temperature for I–III; acetonitrile–25 mM KH2PO4–acetic acid (45 + 55 + 0.2, v/v/v), flowing at a rate of 1.5 mL/min and detection at 234 nm at ambient temperature, was used for IV and V. Methyl paraben was used as an internal standard. The detection limits were 0.35 (I), 5.0 (II), 1.5 (III), 3.0 (IV), and 2.0 g/mL (V). The method was accurate (mean recovery 98 ± 2%, n = 4) and precise (coefficient of variation <5%, n = 5). The proposed method is rapid and sensitive and, therefore, suitable for the routine control of these ingredients in multicomponent dosage forms.

Rapid Method for the Determination of Vitamins A and E in Foods Using Ultra-High-Performance Liquid Chromatography

2012 ◽  
Vol 95 (2) ◽  
pp. 517-522 ◽  
Author(s):  
You -Shin Shim ◽  
Ki-Jin Kim ◽  
Dongwon Seo ◽  
Masahito Ito ◽  
Hiroaki Nakagawa ◽  
...  
Keyword(s):  
Particle Size ◽  
High Performance Liquid Chromatography ◽  
Rapid Method ◽  
High Performance ◽  
Hplc Analysis ◽  
Hplc Method ◽  
The Novel ◽  
Hplc Separation ◽  
Interday Precision

Abstract A rapid and novel ultra-HPLC (u-HPLC) method for the determination of vitamins A (retinol) and E (α-, γ-, and δ-tocopherol) in foods was validated in terms of its precision, accuracy, and linearity. The u-HPLC separation was performed on an RP C18 column (particle size 2 μm, id 2 mm, and length 75 mm), followed by fluorescence detection. The recovery of retinol was more than 84.58%; the LOD and LOQ of the u-HPLC analysis were 0.015 and 0.045 mg/kg, respectively. The intraday and interday precision was less than 9.12%. The recoveries of α-, γ-, and δ-tocopherol were more than 81.37%; the LOD and the LOQ were 0.014, 0.002, and 0.001 mg/kg and 0.042, 0.005, and 0.004 mg/kg, respectively. All calibration curves had good linearity (r2 = 0.99) within the test ranges. The novel, rapid method coupled to u-HPLC can provide significant improvements in the speed, sensitivity, and resolution compared with a conventional HPLC method.

scholarly journals Challenges of HPLC Method Development and Validation for the Assay of Bemotrizinol from Complex Matrix in Cosmeceutical Preparation

2020 ◽  
Vol 11 (03) ◽  
pp. 310-316
Author(s):  
Kallol S Jana ◽  
Beduin Mahanti
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Linear Regression Analysis ◽  
Cost Effective ◽  
Analysis Data ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Relative Standard

A simple high performance liquid chromatography (HPLC) method was developed for the assay of bemotrizinol (Tinosorb-S) from the complex pharmaceutical cosmetics matrix. Unlike the existing methods, the proposed mobile phase used in this method is very simple and excluding buffer. The use of buffer reducing column longevity and also a time-consuming process which increases the cost of analysis. To overcome all the referred problems, the present article was developed and validated as per International Council for Harmonization (ICH) guidelines. The reverse-phase chromatography was performed on Shimadzu model no. SPD-M10A VP with LC solution software, μBondapack (3.9 × 300 mm, 10-micron particle size) column with methanol (100%) as mobile phase at a flow rate 2.5 mL per minutes and UV detection at 254 nm. The retention time of bemotrizinol was found in 17.599 minutes, and the linear regression analysis data for the calibration plots showed a good linear relationship in the concentration range 70 to 130 μg/mL. The value of the correlation coefficient, slope, and intercept were 0.996, 7,715, and 15,320, respectively. The limit of quantification (LoQ) and limit of detection (LoD) were found to be 1.32 and 0.44, respectively. The relative standard deviation (RSD) for intra-day sample A 1.0858, sample B 0.8859, and inter-day sample A 0.9921, sample B 0.967 which were found to be lesser than 2%. The developed method was validated with regard to linearity, accuracy, precision, selectivity, and robustness, and the method was found to be simple, cost-effective, precise, accurate, linear, and specific for the successful identification and determination of bemotrizinol in pharmaceutical cosmetic preparation.

scholarly journals Stability-Indicating High-Performance Thin-Layer Chromatographic Method for Quantitative Determination of Omeprazole in Capsule Dosage Form

2010 ◽  
Vol 93 (3) ◽  
pp. 787-791 ◽  
Author(s):  
Preeta Jha ◽  
Rabea Parveen ◽  
Suroor A Khan ◽  
Ozair Alam ◽  
Sayeed Ahmad
Keyword(s):  
Quantitative Determination ◽  
Mobile Phase ◽  
High Performance ◽  
Dosage Form ◽  
Linear Regression Analysis ◽  
Analysis Data ◽  
Stability Testing ◽  
Mean Values ◽  
Stability Indicating

Abstract A novel HPTLC method has been developed and validated for quantitative determination of omeprazole (OPZ) in capsule dosage form. The method was validated according to the International Conference on Harmonization guidelines for accuracy, precision, linearity, specificity, and robustness. HPTLC aluminum sheets precoated with silica gel 60F254 were used as the stationary phase and chloroformmethanol (9 + 1) as the mobile phase. The mobile phase was found to give compact bands for OPZ (Rf value of 0.39 0.12) in densitometric analysis in the absorbance mode at 302 nm. The linear regression analysis data for the calibration plots showed good linearity (r2 = 0.997) with respect to peak area in the concentration range 503000 ng/band. The mean values of the slope and intercept were 9.896 0.0753 and 1870.761 16.866, respectively. The method was also applied for stability testing of OPZ in different stress conditions and found to be accurate, linear, precise, robust, specific, and stability indicating. The method proposed can be used for QC and stability testing of different dosage forms such as tablets and capsules, as well as for bulk drug analysis of OPZ.

Separation and Determination of Some Aromatic Sulfones by Reversed-Phase High-Performance Liquid Chromatography

1994 ◽  
Vol 59 (3) ◽  
pp. 569-574 ◽  
Author(s):  
Josef Královský ◽  
Marta Kalhousová ◽  
Petr Šlosar
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Reversed Phase ◽  
Uv Spectra ◽  
Optimum Conditions ◽  
Linear Calibration ◽  
Technical Grade

The reversed-phase high-performance liquid chromatography of some selected, industrially important aromatic sulfones has been investigated. The chromatographic behaviour of three groups of aromatic sulfones has been studied. The optimum conditions of separation and UV spectra of the sulfones and some of their hydroxy and benzyloxy derivatives are presented. The dependences of capacity factors vs methanol content in mobile phase are mentioned. The results obtained have been applied to the quantitative analysis of different technical-grade samples and isomer mixtures. For all the separation methods mentioned the concentration ranges of linear calibration curves have been determined.

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