scholarly journals A rapid spectrophotometric determination of imidacloprid in selected commercial formulations in the presence of 6-chloronicotinic acid

2009 ◽  
Vol 74 (12) ◽  
pp. 1455-1465 ◽  
Author(s):  
Valéria Guzsvány ◽  
Zsigmond Papp ◽  
Sanja Lazic ◽  
Ferenc Gaál ◽  
Luka Bjelica ◽  
...  

A simple first-order derivative spectrophotometric method was developed for the simultaneous determination of imidacloprid and 6-chloronicotinic acid (6-CNA). By using the zero-crossing approach, imidacloprid was determined at 249 nm and 6-CNA at 236 nm with detection limits of 0.32 and 0.17 ?g mL-1, respectively, and relative standard deviations not exceeding 1.2 % in the case of model systems. The proposed method was applied for the determination of imidacloprid and 6-CNA in commercial formulations. A conventional spectrophotometric method (at 270 nm) was also employed for the determination of the content of imidacloprid in the same commercial formulations. The results of the developed spectrophotometric methods were in good agreement with those obtained by the high-performance liquid chromatographic method.

2008 ◽  
Vol 91 (4) ◽  
pp. 756-761 ◽  
Author(s):  
Satish A Patel ◽  
Arun M Prajapati ◽  
Paresh U Patel ◽  
Natubhai J Patel ◽  
Jayesh B Vaghmasi

Abstract The manuscript describes validated reversed-phase column high-performance liquid chromatographic (RP-HPLC) and first-derivative UV spectrophotometric methods for the estimation of levofloxacin (LFX) and ornidazole (ORNI) in combined dosage forms. The RP-HPLC separation was achieved on a Phenomenex C18 column (250 mm 4.6 mm id, 5 m) using KH2PO4 buffer (pH 6.8)methanolacetonitrile (70 + 15 + 15, v/v/v) mobile phase at a flow rate of 1.5 mL/min and ambient temperature (25 2<sup/>C). Quantification was achieved with photodiode array detection at 295 nm over the concentration range of 110 g/mL for both LFX and ORNI, with mean recovery of 101.7 0.23 and 99.23 1.57, respectively, by the RP-HPLC method. The derivative spectrophotometric method was based on the determination of both the drugs at their respective zero crossing point (ZCP). The first-order derivative spectra were obtained at N =1 (scaling factor), = 2.0 nm (wavelength interval), and the determinations were made at 310 nm (ZCP of ORNI) for LFX and 295 nm (ZCP of LFX) for ORNI over the concentration range of 240 g/mL for both LFX and ORNI. Mean recovery was 99.46 0.96 and 100.9 0.72, respectively, by the first-derivative UV spectrophotometric method. Standard and sample solutions were prepared with methanol as the solvent in both of the methods. These methods were found to be simple, accurate, precise, and sensitive and were applicable for the simultaneous determination of LFX and ORNI in combined dosage forms.


2009 ◽  
Vol 92 (2) ◽  
pp. 404-409 ◽  
Author(s):  
Abdalla A Elshanawane ◽  
Samia M Mostafa ◽  
Mohamed S Elgawish

Abstract A high-performance liquid chromatographic method was developed for the simultaneous determination of 2 ternary mixtures containing amiloride hydrochloride, atenolol, hydrochlorothiazide, and chlorthalidone used in hypertension therapy. The use of cyanopropyl column results in satisfactory separation of both mixtures. The mobile phase consisted of 10 mM KH2PO4 buffer (pH 4.5) and methanol in a ratio of (75 25 v/v), at a flow rate of 1 mL/min. UV detector was operated at 275 nm. Calibration graphs were linear in the concentration ranges of 210, 20200, 10100, and 550 g/mL for amiloride hydrochloride, atenolol, hydrochlorothiazide, and chlorthalidone, respectively. Intraday and interday precision values (relative standard deviation) were <1.13 for mixture I (amiloride hydrochloride, atenolol, chlorthalidone), and <0.93 for mixture II (amiloride hydrochloride, atenolol, hydrochlorothiazide). The method was successfully applied for the determination of the 2 combinations in laboratory-prepared mixtures and commercial pharmaceutical formulation with high accuracy and precision. Statistical comparison of the results with those of the published methods showed excellent agreement and indicates no significant difference between them.


2013 ◽  
Vol 9 (2) ◽  
pp. 26-29 ◽  
Author(s):  
AK Hemanth Kumar ◽  
V Sudha ◽  
Geetha Ramachandran

A high performance liquid chromatographic method for determination of rifabutin in human plasma was  developed. The method involved deproteinisation of the sample with acetonitrile and analysis of the  supernatant using a reversed-phase C18 column (250mm) and UV detection at a wavelength of 265nm.  The assay was specific for rifabutin and linear from 0.025 to 10.0μg/ml. The relative standard deviation  of intra- and inter-day assays was lower than 10%. The method was able to remove interfering materials  in plasma, yielding an average recovery of rifabutin from plasma of 101%. Due to its simplicity, the assay  can be used for pharmacokinetic studies of rifabutin. SAARC Journal of Tuberculosis, Lung Diseases & HIV/AIDS; 2012; IX(2) 26-29 DOI: http://dx.doi.org/10.3126/saarctb.v9i2.7975


2008 ◽  
Vol 91 (1) ◽  
pp. 67-72 ◽  
Author(s):  
Juliana Sippel ◽  
Letcia L Sfair ◽  
Elfrides E S Schapoval ◽  
Martin Steppe

Abstract A new high-performance liquid chromatographic method was developed and validated for clopidogrel determination in pharmaceutical formulations. The system consisted of an ACE 5 octadecylsilane (C18; 150 4.6 mm id), 5.0 m particle size column; methanol0.1 triethylamine (75 + 25, v/v), pH 5.3, mobile phase at a flow rate of 1.2 mL/min; and a diode array detector set at 220 nm. Specificity, linearity, precision, accuracy, and robustness were the parameters evaluated. The retention time for clopidogrel was 6.8 min. To estimate specificity, an aqueous sample solution was subjected to degradation by ultraviolet light and by acid, alkaline, and oxidation media. The peaks of degradation products did not interfere with the compound signal, and there was no interference when a placebo solution was analyzed. Linearity over a concentration range of 10.0 to 90.0 g/mL was shown (correlation coefficient = 0.9998). Low values of relative standard deviation indicated the adequate intraday and interday precision. The average recovery was found as 99.16. In the robustness test, small modifications to the mobile phase composition did not affect the determination of clopidogrel. The proposed method proved to be simple, fast, and cost efficient for the intended use.


2012 ◽  
Vol 2012 ◽  
pp. 1-6 ◽  
Author(s):  
Chang-Seob Seo ◽  
Jung Hoon Kim ◽  
Hyeun-Kyoo Shin

A simple, rapid, and accurate high-performance liquid chromatographic method was applied to the quantitative analysis of six components of a traditional herbal formulation, Insampaedok-san (ISPDS): liquiritin (1), ferulic acid (2), naringin (3), hesperidin (4), neohesperidin (5), and glycyrrhizin (6). The six components were separated within 35 min using a Gemini C18 column maintained at 40°C. The mobile phase was composed of 1.0% (v/v) aqueous acetic acid (A) and 1.0% (v/v) acetic acid in acetonitrile (B) by gradient elution. The flow rate was 1.0 mL/min and the detector was a photodiode array (PDA) set at 254, 280, and 320 nm. The calibration curves showed good linearity (R2=1.0000) for different concentration ranges. The recovery of each component was in the range of 92.62%–105.96%, with a relative standard deviation (RSD) of less than 4.0%. The RSDs for intra- and interday precision were 0.04%–1.70% and 0.06%–2.56%, respectively. The concentration of each of the six components of ISPDS was in the range 0.72–9.88 mg g−1.


2008 ◽  
Vol 91 (1) ◽  
pp. 52-58 ◽  
Author(s):  
Jlia Menegola ◽  
Martin Steppe ◽  
Elfrides E S Schapoval

Abstract Column high-performance liquid chromatographic (LC) and UV spectrophotometric methods for the quantitative determination of citalopram, a potent and selective serotonin reuptake inhibitor, in tablets were developed. The parameters linearity, precision, accuracy, specificity, robustness, limit of detection, and limit of quantitation were studied according to International Conference on Harmonization guidelines. Chromatography was carried out by the reversed-phase technique on an ACE C18 column with a mobile phase composed of 0.30 triethylamine solutionacetonitrile (55 + 45, v/v) adjusted to pH 6.6 with 10 ortho-phosphoric acid at a flow rate of 1.0 mL/min and 25C. The UV spectrophotometric method was performed at 239 nm. The linearity of the LC method was in the range of 10.0070.00 g/mL, and 2.5017.50 g/mL for the UV spectrophotometric method. The interday and intraday assay precision was <1.5 (relative standard deviation) for the LC and UV spectrophotometric methods. The recoveries were in the range 100.70101.35 for the LC method and 98.4898.65 for the UV spectrophotometric method. Statistical analysis by Student's t-test showed no significant difference between the results obtained by the 2 methods. The proposed methods are highly sensitive, precise, and accurate and can be used for the reliable quantitation of citalopram in tablets.


Author(s):  
Kohei Togami ◽  
Kenta Fukuda ◽  
Kotaro Yamaguchi ◽  
Sumio Chono ◽  
Hitoshi Tada

Objective: In this study, a facile and sensitive high-performance liquid chromatographic method for determination of nintedanib in rat plasma was developed and validated.Methods: After plasma protein was precipitated by addition of acetonitrile, the supernatant underwent centrifugation. An aliquot was then injected into a high-performance liquid chromatographic system with a Mightysil RP-18 GP II ODS column (250 × 3.0 mm, length by inner diameter, 5-μm particle size) maintained at 50 °C. A mobile phase mixture of 20 mmol phosphate buffer (pH 3.0) and acetonitrile (7:3, v/v) was used at a flow rate of 0.6 mL/min, with UV detection at a wavelength of 390 nm for isocratic separation and detection of nintedanib, its main metabolite (BIBF1202), and p-nitrophenol as an internal standard.Results: The quantitative range of nintedanib concentration in this method was 12.5–400 ng/ml, and the calibration curves were linear. The intra-and inter-day accuracy values (relative errors) were in the range of −3.65%–4.00% and −3.65%–3.64%, respectively. The intra-and inter-day precision values (relative standard deviations) were<5.9% and 8.36%, respectively. The method was successfully applied to a pharmacokinetic analysis of nintedanib in rats after intravenous administration.Conclusion: In this study, a rapid, sensitive, and simple HPLC-UV method for the quantitation of nintedanib in rat plasma was developed and validated. The method was shown to be accurate and precise and was successfully applied to a pharmacokinetic study.


2008 ◽  
Vol 91 (4) ◽  
pp. 744-749 ◽  
Author(s):  
Islam Ullah Khan ◽  
Shahzad Sharif ◽  
Muhammad Ashfaq ◽  
Muhammad Nadeem Asghar

Abstract A simple, precise, and sensitive high-performance liquid chromatographic method was developed and validated for the simultaneous determination of potassium clavulanate and cefixime in synthetic mixture form. The analytes were separated on a C18 column by using 0.03 M disodium hydrogen phosphate buffer (pH 6.5)methanol (84 + 16, v/v) as the mobile phase with detection at 220 nm. The method exhibited high sensitivity and good linearity in the concentration ranges of 12.562.5 and 20100 g/mL for potassium clavulanate and cefixime, respectively. The total run time for the 2 components was &lt;8 min, and the average recovery was &gt;101.5 with a relative standard deviation of &lt;1.0. The proposed method was validated according to guidelines of the International Conference on Harmonization by evaluation of linearity, recovery, selectivity, robustness, limits of detection and quantitation, and within- and between-day precision. The results obtained for the synthetic mixture show that the method is highly precise and accurate for the simultaneous determination of potassium clavulanate and cefixime.


2010 ◽  
Vol 7 (3) ◽  
pp. 827-832 ◽  
Author(s):  
R. Kalaichelvi ◽  
B. Thangabalan ◽  
D. Srinivasa Rao

A rapid, simple and validated reversed-phase high-performance liquid chromatographic method has been developed for analysis of aripiprazole in tablet dosage form. Aripiprazole was separated on an ODS analytical column with a 40:60 (v/v) mixture of acetonitrile and triethanolamine buffer (5 mM, pH 3.5 ± 0.05 adjusted by addition of 85% phosphoric acid) as mobile phase at a flow rate of 1.5 mL min-1. The effluent was monitored by UV detection at 254 nm. Calibration plots were linear in the range of 20 to 60 µg mL-1and the LOD and LOQ were 0.411 and 1.248 µg mL-1, respectively. The high recovery and low relative standard deviation confirm the suitability of the method for routine quality control determination of aripiprazole in tablets.


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