scholarly journals A simple HPLC method containing greener modifier and slighter temperature elevated for simultaneous determination of three statin drugs in tablets

2021 ◽  
Author(s):  
Wael Alshitari ◽  
Fatimah Al-Shehri ◽  
Deia Abd El-Hady ◽  
Hassan M. Albishri
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Optimal Conditions ◽  
Limit Of Quantification ◽  
Column Temperature ◽  
Pharmaceutical Tablets ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Statin Drugs

AbstractStatins drugs are thought to be among the most prescribed drugs worldwide for the treatment of hypercholesterolaemia. A simple and reliable RP-HPLC method has been successfully employed for simultaneously separating and qualifying three statin drugs including atorvastatin, rosuvastatin and simvastatin in pharmaceutical tablets. The optimal conditions were mobile phase 50:50 (v/v) (formic acid pH 2.50: ETOH), column temperature 40.00 °C, detection wavelength 238.00 nm, and flow rate 1.00 mL/min. The proposed method has been validated based on the ICH guidelines in terms of linearity, precision, accuracy, and limit of detection and limit of quantification. The linear range investigated 2.0–80.0, 4.0–100.00, and 12.00–120.00 µg/mL for rosuvastatin, atorvastatin and simvastatin respectively with coefficients of determination (R2) within the range of 0.9993–0.9995. The LOD and LOQ for rosuvastatin, atorvastatin and simvastatin were (1.57, 4.76 µg/mL), (1.87, 5.66 µg/mL), (3.46, 10.49 µg/mL) respectively. In addition, in order to evaluate the feasibility of the method developed, it was employed towards the quantification of the pharmaceutical tablets for the analytes investigated and excellent recovery was obtained.

scholarly journals Development and Validation of a Rapid RP-HPLC Method for the Estimation of Esmolol Hydrochloride in Bulk and Pharmaceutical Dosage Forms

2010 ◽  
Vol 7 (3) ◽  
pp. 807-812 ◽  
Author(s):  
Vanita Somasekhar ◽  
D. Gowri Sankar
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Detector Response ◽  
Reverse Phase Hplc ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Development And Validation

A reverse phase HPLC method is described for the determination of esmolol hydrochloride in bulk and injections. Chromatography was carried on a C18column using a mixture of acetonitrile, 0.05 M sodium acetate buffer and glacial acetic acid (35:65:3 v/v/v) as the mobile phase at a flow rate of 1 mL/min with detection at 275 nm. The retention time of the drug was 4.76 min. The detector response was linear in the concentration of 1-50 μg/mL. The limit of detection and limit of quantification was 0.614 and 1.86 μg/mL respectively. The method was validated by determining its sensitivity, linearity, accuracy and precision. The proposed method is simple, economical, fast, accurate and precise and hence can be applied for routine quality control of esmolol hydrochloride in bulk and injections.

scholarly journals Reverse Phase Chiral HPLC Method for Enantiomeric Excess Determination of 2-Aminobutanamide

2019 ◽  
Vol 32 (1) ◽  
pp. 69-72
Author(s):  
T. Naga Jhansi ◽  
D. Pavan Kumar ◽  
Nagaraju Rajana ◽  
D. Jayadeep Kumar ◽  
G. Nageswara Rao
Keyword(s):  
Limit Of Detection ◽  
Enantiomeric Excess ◽  
Hplc Method ◽  
Chiral Hplc ◽  
Reverse Phase ◽  
Limit Of Quantification ◽  
Perchloric Acid Solution ◽  
Column Temperature ◽  
Isomer Content

A reverse phase chiral HPLC method was developed for the determination of (R)-2-aminobutanamide isomer content in (S)-2-amino-butanamide key starting material for levetiracetam drug substance by using a CROWNPAK CR (+) column. Perchloric acid solution (0.05 %) was used as mobile phase and the flow rate was finalized as 0.3 mL/min. UV detection wavelength was 200 nm and column temperature was set as 15 ºC. The limit of detection and limit of quantification were 0.0002 mg/mL and 0.0005 mg/mL, respectively. The linearity calibration curve of (R)-2-aminobutanamide was shown good from the range of 0.0005 mg/mL to 0.004 mg/mL. The recovery of (R)-2-aminobutanamide isomer was between the range of 93 to 106 % in presence of (S)-2-aminobutanamide. The method was validated and found to be precise, accurate and robust. The method can be used for determination of (R)-2-aminobutanamide in presence of (S)-2-aminobutanamide, which is the key intermediate for preparation of levetiracetam. This method was validated in as per ICH Q2 (R1) and USP validation of compendial methods (1225).

scholarly journals Development and Validation of RP-Chiral HPLC Method for Determination of (R)-Enantiomer Excess Content in Efavirenz

2020 ◽  
Vol 32 (9) ◽  
pp. 2208-2212
Author(s):  
CH. RAMESH ◽  
DHARMASOTH RAMA DEVI DEVI ◽  
M.N.B. SRINIVAS ◽  
S. RADHA KRISHNA ◽  
NAGARAJU RAJANA ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Chiral Hplc ◽  
Reverse Phase ◽  
Limit Of Quantification ◽  
Column Temperature ◽  
Enantiomer Excess ◽  
Development And Validation ◽  
Methyl Phenyl

simple, specific, linear, accurate and precise reverse phase chiral HPLC method was developed for the separation of efavirenz enantiomers by using the Lux Amylose-2 column containing amylose tris(5-chloro-2-methyl phenyl carbamate) as a stationary phase. The mobile phase consists of 0.1 % formic acid in water and acetonitrile (55:45, v/v). The flow rate was kept at 1.0 mL/min and the detection wavelength used 252 nm and the column temperature was set at 25 ºC. The limit of detection was 0.01 mg/mL and the limit of quantification was 0.04 mg/mL. The linearity calibration curve of (R)-enantiomer was shown well from the range of 0.04 mg/mL to 0.4 mg/mL. The values of the correlation coefficient were 0.999 and 0.999 for (R)-enantiomer and (S)-efavirenz, respectively. The percentage recoveries of (R)-enantiomer from efavirenz drug substance were ranged from 93.5% to 107.5%. The results demonstrated that developed RP-chiral HPLC method was simple, precise, robust and applicable for the estimation of (R)-enantiomer in efavirenz API. This method was validated in as per ICH Q2 (R1) and USP validation of compendial methods <1225>.

scholarly journals Development and validation of novel RP-UPLC method for estimation of atropine sulphate in pharmaceutical dosage form

2013 ◽  
Vol 19 (3) ◽  
pp. 333-337 ◽  
Author(s):  
A.C. Arvadiya ◽  
P.P. Dahivelker
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Atropine Sulphate ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Column Temperature ◽  
Ich Guidelines ◽  
Development And Validation

A simple, precise, accurate, sensitive and repeatable RP-UPLC method was developed for quantitative determination of atropine sulphate in pharmaceutical dosage form. The method was developed by using C18 column Hiber HR Purospher Star (100mm?2.1mm id, 2?m particle size) as stationary phase with Phosphate Buffer: Acetonitrile (87:13, %v/v) as a mobile phase, pH was adjusted to 3.5 by ortho-phosphoric acid at a flow rate of 0.5 mL/min and column temperature maintained at 30?C. Quantification of eluted compound was achieved with PDA detector at 210 nm. Atropine sulphate followed linearity in concentration range of 2.5-17.5 ?g/mL with r2=0.9998 (n=6). Limit of detection (LOD) and limit of quantification (LOQ) values were 0.0033 and 0.0102 ?g/mL for atropine sulphate. The validation study is carried out as per International Conference on Harmonization (ICH) guidelines. This method was successfully applied for estimation of atropine sulphate in pharmaceutical formulation.

scholarly journals Spectrophotometric and RP-HPLC Methods for Determining Cefotaxime Sodium in Pharmaceutical Preparations

2020 ◽  
Vol 32 (6) ◽  
pp. 1314-1320
Author(s):  
Lamya A. Sarsam ◽  
Salim A. Mohammed ◽  
Sahar A. Fathe
Keyword(s):  
Limit Of Detection ◽  
Phosphate Buffer Solution ◽  
Pharmaceutical Preparations ◽  
Molar Absorptivity ◽  
Hplc Method ◽  
Buffer Solution ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Relative Standard

A rapid, simple and sensitive spectrophotometric and RP-HPLC methods have been developed for the quantitative determination of cefotaxime-Na in both pure and dosage forms. The spectrophotometric method was based on diazotization of cefotaxime-Na and then coupling with 8-hydroxyquinoline in an alkaline medium. The resulting azo dye exhibited maximum absorption at 551 nm with a molar absorptivity of 0.597 × 104 L mol-1 cm-1. Beer′s law was obeyed over the range 10-700 μg/25 mL (i.e. 0.4-28.0 ppm) with an excellent determination coefficient (R2 = 0.9993). The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.0194 and 0.3765 μg mL-1, respectively. The recoveries were obtained in the range 97.3-102.5% and the relative standard deviation (RSD) was better than ± 1.56. The HPLC method has been developed for the determination of cefotaxime-Na. The analysis were carried out on a C18 column and a mobile phase composed of acetonitrile and phosphate buffer solution (0.024M KH2PO4 and 0.01M H3PO4) at pH 3.5 in the ratio of 60:40 (v:v), with a flow rate of 1.0 mL min-1 and UV detection at 258 nm. The proposed method showed good linearity (in a range of concentration 1.0-200 μg mL-1. The recovery percent and a relative standard deviations were found in the range 96 to 104.8% and ± 0.017 to ± 0.031%, respectively. Both methods were applied successfully to the assay of cefotaxime-Na in commercial injection preparations.

DEVELOPMENT AND VALIDATION OF RP HPLC METHOD FOR THE ESTIMATION OF SOFOSBUVIR IN BULK, TABLET AND INDUSTRIAL WASTE WATER

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (06) ◽  
pp. 59-66
Author(s):  
V Dhanunjayachary ◽  
◽  
V.L.S. Likhitha ◽  
Sri K. Vijaya ◽  
M. A Madhuri
Keyword(s):  
Industrial Waste ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
System Suitability ◽  
Limit Of Quantitation ◽  
Development And Validation

The study was aimed at development and validation of RP-HPLC method for estimation of sofosbuvir in bulk, pharmaceutical dosage form and pharmaceutical industrial waste. The chromatographic separation was performed on Agilent Syncronis C 18 (100 mm × 4.6 mm, 5μm) column, with a mobile phase comprising of a mixture of methanol: acetonitrile: water (45:30:25 v/v/V). The flow rate was 1.0 mL/min with detection at 260 nm. Retention time of sofosbuvir was found to be 2.040 min. As per ICH guidelines, the method was validated for linearity, accuracy, limit of detection, limit of quantitation, precision, robustness and system suitability. Linearity was found to be in the range of 4-24 μg/mL with regression equation y = 675284.x + 49120 and correlation coefficient 0.999. The low % RSD values indicate the method to be accurate and precise. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.046 and 0.1400 μg/mL, respectively. The % recovery of tablets was found to be in the range of 99.9– 101.3%. It can be concluded that this validated HPLC method is easy, precise, accurate, sensitive and selective for estimation of sofosbuvir in bulk, tablet and applicable for analyses of in pharmaceutical industrial waste.

scholarly journals Development, Validation and Application of RP-HPLC Method: Simultaneous Determination of Antihistamine and Preservatives with Paracetamol in Liquid Formulations and Human Serum

2016 ◽  
Vol 10 (1) ◽  
pp. 33-43 ◽  
Author(s):  
Najmul Hasan ◽  
Mathurot Chaiharn ◽  
Umair Ali Toor ◽  
Zulfiqar Ali Mirani ◽  
Ghulam Sajjad ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Oral Solution ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Physiological Fluid ◽  
Development And Validation

In this article we describe development and validation of stability indicating, accurate, specific, precise and simple Ion-pairing RP-HPLC method for simultaneous determination of paracetamol and cetirizine HCl along with preservatives i.e. propylparaben, and methylparaben in pharmaceutical dosage forms of oral solution and in serum. Acetonitrile: Buffer: Sulfuric Acid (45:55:0.3 v/v/v) was the mobile phase at flow rate 1.0 mL min-1 using a Hibar® Lichrosorb® C18 column and monitored at wavelength of 230nm. The averages of absolute and relative recoveries were found to be 99.3%, 99.5%, 99.8% and 98.7% with correlation coefficient of 0.9977, 0.9998, 0.9984, and 0.9997 for cetirizine HCl, paracetamol, methylparaben and Propylparaben respectively. The limit of quantification and limit of detection were in range of 0.3 to 2.7 ng mL-1 and 0.1 to 0.8 ng mL-1 respectively. Under stress conditions of acidic, basic, oxidative, and thermal degradation, maximum degradation was observed in basic and oxidative stress where a significant impact was observed while all drugs were found almost stable in the other conditions. The developed method was validated in accordance with ICH and AOAC guidelines. The proposed method was successfully applied to quantify amount of paracetamol, cetirizine HCl and two most common microbial preservatives in bulk, dosage form and physiological fluid.

scholarly journals A simple isocratic RP-HPLC method for quality control of oseltamivir capsules

2012 ◽  
Vol 31 (2) ◽  
pp. 205
Author(s):  
Agim Ameti ◽  
Jasmina Slavkovska ◽  
Katerina Starkoska ◽  
Zorica Arsova-Sarafinovska
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Sample Treatment ◽  
Limit Of Quantification ◽  
Elution Time ◽  
Rp Hplc

A simple isocratic reversed-phase high performance liquid chromatographic (RP-HPLC) method was developed for determination of oseltamivir active pharmaceutical ingredient (API) in bulk drug and pharmaceuticals. The separation was achieved on a Purospher STAR® RP – 18e column with a mobile phase consisting of methanol- 0.02 mol l-1 phosphate buffer, pH 5, 50:50 (v/v). Chromatographic results demonstrated the specificity of the method for determination of oseltamivir in presence of degradation products generated in studies of forced decomposition. The limit of detection (LOD) and limit of quantification (LOQ) for oseltamivir phosphate were 0,0162 μg ml-1 and 0,0491 μg ml-1, respectively. The advantages of this method include simple sample treatment and short elution time (less than 6 min). Furthermore, using methanol instead of acetonitrile in a mobile phase composition considerably reduces the laboratory expenses, still retaining adequate sensitivity for routine analysis as well as for evaluation of potentially counterfeit Tamiflu® products. 

DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR THE ESTIMATION OF RAMOSETRON HYDROCHLORIDE IN BULK AND TABLETS

INDIAN DRUGS ◽  
2012 ◽  
Vol 49 (07) ◽  
pp. 54-57
Author(s):  
P. Sathyanarayana ◽  
◽  
M Vijayalakshmi ◽  
B. N. V Ravi Kumar
Keyword(s):  
Flow Rate ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Development And Validation ◽  
High Degree ◽  
Isocratic Mode

A RP-HPLC method was developed and validated for the determination of ramosetron hydrochloride in pharmaceutical formulation as per ICH and FDA guidelines. The method was carried out on a Phenomenex RP-C18 column using a mixture of methanol and water (95:5) in an isocratic mode. The flow rate is 0.8 mL/min and the detection was done at 302 nm. The linearity range was observed in the range of 1-6 mcg/mL. The accuracy of the method was found to be 99.0 to 99.5% and %RSD was found to be less than 2% indicating high degree of accuracy and precision for the proposed HPLC method. Limit of detection and limit of quantification of the method were found to be 0.028 and 0.0851 mcg/mL respectively.

NEW STABILITY INDICATING METHOD FOR ESTIMATION OF PURITY OF FLIBANSERIN ACTIVE PHARMACEUTICAL INGREDIENT

INDIAN DRUGS ◽  
2020 ◽  
Vol 57 (04) ◽  
pp. 40-44
Author(s):  
Yik-Ling Chew ◽  
◽  
Hon-Kent Lee ◽  
Subrahmanya Lokesh Bontha Venkata
Keyword(s):  
Ammonium Acetate ◽  
Limit Of Detection ◽  
Sexual Interest ◽  
Active Pharmaceutical Ingredient ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Rp Hplc ◽  
Ich Guidelines

Flibanserin has been recently approved by the USFDA for treating female sexual interest disorder. It is currently not included in any of the Pharmacopoeias. No stability indicating method information about flibanserin has been reported in the literature. Flibanserin stock solution (1 mg/mL) was prepared and serially diluted (concentration ranged 1-20 μg/mL). Flibanserin solutions (1-20 μg/mL) were analysed using RP-HPLC under isocratic elution of mobile phase acetonitrile and ammonium acetate (60:40; V/V) at 1 mL/minute. This HPLC method was validated for linearity, accuracy, precision, robustness, limit of detection (LOD) and limit of quantification (LOQ), according to ICH guidelines. Results showed that the method developed has promising linearity (r2= 0.9993), accuracy, precision (0.92-1.61%), robustness, LOD and LOQ. The developed HPLC method for evaluation of flibanserin was found reliable, precise, sensitive, accurate and repeatable for routine analysis and quality control of flibanserin. It is suitable to be used as stability indicating method in pharmaceutical analysis.

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