A Validated RP-HPLC Method for the Estimation of Quetiapine in Bulk and Pharmaceutical Formulations

A new, simple, specific, sensitive, rapid, accurate and precise RP-HPLC method was developed for the estimation of quetiapine in bulk and pharmaceutical formulations. Quetiapine was chromatographed on a reverse phase C18Waters column (75x4.6 mm I.D., particle size 3.5 μm) in a mobile phase consisting of phosphate buffer (pH 3.0 adjusted with orthophosphoric acid) and acetonitrile in the ratio 40:60 v/v. The mobile phase was pumped at a flow rate of 0.8 mL/min with detection at 291 nm. The detector response was linear in the concentration of 20-120 μg/mL. The limit of detection and limit of quantitation was found to be 0.2 and 0.75 μg/mL, respectively. The intra and inter day variation was found to be less than 1%. The mean recovery of the drug from the solution was 99%. The proposed method is simple, fast, accurate, precise and reproducible hence, it can be applied for routine quality control analysis of quetiapine in bulk and pharmaceutical formulations.

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VALIDATION OF PROPOSED RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF FENPIVERINIUM BROMIDE AND PITOFENONE HCL

INDIAN DRUGS ◽

10.53879/id.51.07.10114 ◽

2014 ◽

Vol 51 (07) ◽

pp. 39-45

Author(s):

S.V Nagpure ◽

◽

S.V Deshmane ◽

K.R. Biyani

Keyword(s):

Limit Of Detection ◽

Pharmaceutical Formulations ◽

Hplc Method ◽

Simultaneous Estimation ◽

Control Analysis ◽

Quality Control Analysis ◽

Rp Hplc ◽

Limit Of Quantitation ◽

Diammonium Hydrogen

A simple, rapid, accurate and precise RP-HPLC method was developed and validated for the determination of fenpiverinium bromide and pitofenone HCl. Separation of the drug was achieved on a reverse phase Thermo Kromasil C18 Column. The method showed a linear response for concentration in the range of 1.2-2.8μg/ml for FVB 6-14 μg/ml for PFH using diammonium hydrogen orthophosphatee buffer pH 7.2: acetonitrile as the mobile phase in the ratio of 55:45, v/v with detection at 220 nm with a flow rate of 1 ml/min and retention time was 3.77min and 7.45 min for FVB and PFH respectively. The method was statistically validated for linearity, accuracy, precision and selectivity.The limit of detection and limit of quantitation was 0.0654 µg/ml and 0.1982 µg/ml for FVB and 0.0927 µg/ml and 0.281 µg/ml for PFH, respectively. In quantitative and recovery studies, % RSD was found less than 2. Due to simplicity, rapidity and accuracy of the method, we believe that the method will be useful for routine quality control analysis of fenpiverinium bromide and pitofenone HCl in pharmaceutical formulations.

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A Validated RP-HPLC Method for the Estimation of Levetiracetam in Bulk and Pharmaceutical Formulations

E-Journal of Chemistry ◽

10.1155/2010/741417 ◽

2010 ◽

Vol 7 (2) ◽

pp. 600-604 ◽

Cited By ~ 5

Author(s):

A. Lakshmana Rao ◽

V. Naga Jahnavi

Keyword(s):

Mobile Phase ◽

High Performance ◽

Limit Of Detection ◽

Pharmaceutical Formulations ◽

High Performance Liquid Chromatographic ◽

Hplc Method ◽

Detector Response ◽

Control Analysis ◽

Limit Of Quantification ◽

Liquid Chromatographic

A rapid and sensitive high performance liquid chromatographic method was developed for the estimation of levetiracetam in bulk and pharmaceutical formulations. Levetiracetam was chromatographed on a reverse phase C18column in a mobile phase consisting of 0.05 M KH2PO4buffer (pH 3.0 adjusted with orthophosphoric acid) and methanol in the ratio 70:30 v/v. The mobile phase was pumped at a flow rate of 1.2 mL/min. with detection at 210 nm. The detector response was linear in the concentration of 20-120 μg/mL. The limit of detection and limit of quantification was found to be 0.0104 and 0.0317 μg/mL, respectively. The intra and inter day variation was found to be less than 1%. The mean recovery of the drug from the solution containing 100 µg/mL was 100.038 μg/mL. The proposed method is simple, fast, accurate, precise and reproducible hence can be applied for routine quality control analysis of levetiracetam in bulk and pharmaceutical formulations.

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Development and Validation of Stability-Indicating RP-HPLC Method for the Estimation of Lenalidomide and its Impurities in Oral Solid Dosage Form

Oriental Journal Of Chemistry ◽

10.13005/ojc/350115 ◽

2019 ◽

Vol 35 (1) ◽

pp. 140-149 ◽

Cited By ~ 1

Author(s):

Somana Siva Prasad ◽

G. V. Krishna Mohan ◽

A. Naga Babu

Keyword(s):

Limit Of Detection ◽

Degradation Products ◽

Pharmaceutical Formulations ◽

Hplc Method ◽

Stability Robustness ◽

Rp Hplc ◽

Mobile Phases ◽

Limit Of Quantitation ◽

Successful Separation ◽

Quality By Design Approach

In this study, a novel, simple and precise RP-HPLC method has been developed for the quantitative analysis of Lenalidomide (LLM) in pharmaceutical formulations using analytical quality by design approach. An X-bridge-C18 column (150 mm × 4.6 mm × 3.5 µ) with mobile phases containing a Potassium dihydrogen orthophosphate anhydrous buffer and methanol in the ratio of (90:10 v/v) and (35:65 v/v) are used for the estimation of LLM and its degradation products. The flow rate of 0.8 mL/min is maintained and all degradation studies are performed at 210 nm using photodiode array (PDA) detector. Method Validation is carried out according to International Council for Harmonisation (ICH) guidelines and the parameters namely; precision, accuracy, specificity, stability, robustness, linearity, limit of quantitation (LOQ) and limit of detection (LOD) are evaluated. The present developed RP-HPLC method shows the purity angle of peaks is less than their threshold angle, signifying that it to be suitable for stability studies. Hence, the developed method can be used for the successful separation of LLM and its impurities in the pharmaceutical dosage formulations.

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RP-HPLC Estimation of Bumetanide and its Impurities in Oral Solid Dosage Form

Asian Journal of Chemistry ◽

10.14233/ajchem.2019.22069 ◽

2019 ◽

Vol 31 (10) ◽

pp. 2215-2221

Author(s):

P. Suresh Kumar ◽

G.V. Krishna Mohan ◽

A. Naga Babu

Keyword(s):

Limit Of Detection ◽

Degradation Products ◽

Drug Product ◽

Pharmaceutical Formulations ◽

Hplc Method ◽

Fixed Dose ◽

Array Detector ◽

Rp Hplc ◽

Photodiode Array Detector ◽

Limit Of Quantitation

A novel and simultaneous stability indicating RP-HPLC method has been developed for quantitative analysis of bumetanide in fixed dose pharmaceutical formulations. Bumetanide and its degradation products are well separated by the Discovery C18, 250 × 4.6 mm, 5 μm column as a stationary phase and (50:50 v/v) of 0.1 % o-phthalaldehyde and acetonitrile as a mobile phase. All the compounds are monitored using photodiode array detector at 254 nm with an isocratic method and the flow rate of 1.0 mL/min was maintained. Validation of method was performed as per International Council for Harmonization (ICH) guidelines and the parameters namely; precision, accuracy, specificity, stability, robustness, linearity, limit of quantitation (LOQ) and limit of detection (LOD) were evaluated. The linearity of the proposed method was found to be 0.315-1.875 μg/mL for bumetanide and its impurities. The developed method is more economical and suitable for laboratory use because of solvent consumption is very less. Hence, the developed method can be used for the determination of bumetanide and its impurities in drug product stability studies and pharmaceutical formulations.

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A Validated RP-HPLC Method for Simultaneous Estimation of Atenolol and Indapamide in Pharmaceutical Formulations

E-Journal of Chemistry ◽

10.1155/2011/121420 ◽

2011 ◽

Vol 8 (3) ◽

pp. 1238-1245 ◽

Cited By ~ 2

Author(s):

G. Tulja Rani ◽

D. Gowri Sankar ◽

P. Kadgapathi ◽

B. Satyanarayana

Keyword(s):

Particle Size ◽

Mobile Phase ◽

Dosage Form ◽

Orthophosphoric Acid ◽

Pharmaceutical Formulations ◽

Hplc Method ◽

Simultaneous Estimation ◽

Rp Hplc ◽

Ich Guidelines

A simple, fast, precise, selective and accurate RP-HPLC method was developed and validated for the simultaneous determination of atenolol and indapamide from bulk and formulations. Chromatographic separation was achieved isocratically on a Waters C18 column (250×4.6 mm, 5 µ particle size) using a mobile phase, methanol and water (adjusted to pH 2.7 with 1% orthophosphoric acid) in the ratio of 80:20. The flow rate was 1 mL/min and effluent was detected at 230 nm. The retention time of atenolol and indapamide were 1.766 min and 3.407 min. respectively. Linearity was observed in the concentration range of 12.5-150 µg/mL for atenolol and 0.625-7.5 µg/mL for indapamide. Percent recoveries obtained for both the drugs were 99.74-100.06% and 98.65-99.98% respectively. The method was validated according to the ICH guidelines with respect to specificity, linearity, accuracy, precision and robustness. The method developed can be used for the routine analysis of atenolol and indapamide from their combined dosage form.

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A Validated RP-HPLC Method for the Determination of Citrinin in Xuezhikang Capsule and otherMonascus-Fermented Products

E-Journal of Chemistry ◽

10.1155/2012/693570 ◽

2012 ◽

Vol 9 (1) ◽

pp. 260-266 ◽

Cited By ~ 2

Author(s):

Li Xue-Mei ◽

Shen Xing-Hai ◽

Xue Lan ◽

Duan Zhen-Wen ◽

Guo Shu-Ren

Keyword(s):

Mobile Phase ◽

Limit Of Detection ◽

Hplc Method ◽

Quantitative Detection ◽

Rp Hplc ◽

Toxic Product ◽

Limit Of Quantitation ◽

Xuezhikang Capsule ◽

Fermented Products

Citrinin is a toxic product usually produced during theMonascusfermentation. The presence of citrinin in xuezhikang capsule has been a concern due to its ingredient which is derived frommonascus-fermented rice. A rapid and sensitive RP-HPLC method with fluorescence detection at λex= 331 nm and λem= 500 nm for analysis of citrinin inMonascus-fermented products was developed to analyze citrinin inMonascus-fermented products. The chromatography was performed with mobile phase containing acidified water and acetonitrile. The calibration curve was linear (r = 0.9999) over a range of 0.0107- 0.537 μg/mL. The limit of detection (LOD) and the limit of quantitation (LOQ) were 0.187 ng/mL and 0.6 ng/mL respectively. The analysis of xuezhikang capsules using the developed method suggested that the product does not contain detectable citrinin and the result has been further confirmed using independent LC-MS/MS analysis. The proposed method has also been applied to analyze 11 samples of otherMonascus-fermented products. The results suggested that there were no detectable citrinin in 4 of the 11 samples, however citrinin with the levels between 0.10-594 ng/kg has been detected in the other 7 samples. It indicates that the proposed method can also be applied to carry out the quantitative detection of citrinin for otherMonascus-fermented products.

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A Validated RP-HPLC Stability Method for the Estimation of Chlorthalidone and Its Process-Related Impurities in an API and Tablet Formulation

International Journal of Analytical Chemistry ◽

10.1155/2020/3593805 ◽

2020 ◽

Vol 2020 ◽

pp. 1-11

Author(s):

Chaitali Kharat ◽

Vaishali A. Shirsat ◽

Yogita M. Kodgule ◽

Mandar Kodgule

Keyword(s):

Mobile Phase ◽

Limit Of Detection ◽

Hplc Method ◽

Buffer Solution ◽

Related Impurities ◽

First Line Therapy ◽

Rp Hplc ◽

Limit Of Quantitation ◽

Bulk Drug ◽

Simultaneous Identification

Low-dose thiazide and thiazide-like diuretics are widely used as first-line therapy for hypertension. Chlorthalidone, a monosulfamyl diuretic, is frequently prescribed in cases of hypertension and congestive heart failure. In this research paper, an improved reverse-phase HPLC method was developed for the simultaneous identification and quantitation of pharmacopoeia-listed and in-house process- and degradation-related impurities of chlorthalidone in bulk drug and formulations. Chromatographic separation was carried out on a C8 column (250 × 4.6 mm; ‘5 μm particle size) at a flow rate of 1.4 mL/min with a 220 nm detection wavelength. Mobile phase A consisted of buffer solution (diammonium hydrogen orthophosphate (10 mM, pH 5.5)) and methanol at a 65 : 35 ratio (v/v), and mobile phase B consisted of buffer solution and methanol at a 50 : 50 ratio (v/v). The API and formulation were subjected to stress conditions such as acid, alkali, oxidation, thermal, and photolytic conditions. Validation studies for the in-house process impurities were performed for specificity, limit of detection (LOD), limit of quantitation (LOQ), linearity, precision, accuracy, and robustness. Thus, an improved RP-HPLC method capable of good separation of all known and unknown impurities with acceptable resolution and tailing factor was developed.

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Optimization and validation of an RP-HPLC method for the estimation of 6-mercaptopurine in bulk and pharmaceutical formulations

Brazilian Journal of Pharmaceutical Sciences ◽

10.1590/s1984-82502014000400015 ◽

2014 ◽

Vol 50 (4) ◽

pp. 793-797 ◽

Cited By ~ 2

Author(s):

Vanita Somasekhar

Keyword(s):

Limit Of Detection ◽

Pharmaceutical Formulations ◽

Hplc Method ◽

Detector Response ◽

Reverse Phase Hplc ◽

Reverse Phase ◽

Limit Of Quantification ◽

Rp Hplc ◽

Accuracy And Precision

A reverse phase HPLC method is described for the determination of 6-mercaptopurine in bulk and tablets. Chromatography was carried on a C18 column using a mixture of acetonitrile and 0.05 mol/L sodium acetate buffer (10:90 v/v) as the mobile phase at a flow rate of 1 mL/min-1 with detection at 324 nm. The retention time of the drug was 3.25 min. The detector response was linear in the concentration of 0.01-5 μg/mL. The limit of detection and limit of quantification were 17 and 52 ng/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 mercaptopurine in bulk and tablets.

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Simultaneous Estimation of Gemcitabine Hydrochloride and Capecitabine Hydrochloride in Combined Tablet Dosage Form by RP-HPLC Method

E-Journal of Chemistry ◽

10.1155/2011/437157 ◽

2011 ◽

Vol 8 (3) ◽

pp. 1212-1217 ◽

Cited By ~ 2

Author(s):

V. Rajesh ◽

B. Anupama ◽

V. Jagathi ◽

P. Sai Praveen

Keyword(s):

Mobile Phase ◽

High Performance ◽

Dosage Form ◽

Limit Of Detection ◽

Hplc Method ◽

Simultaneous Estimation ◽

Gemcitabine Hydrochloride ◽

Rp Hplc ◽

Limit Of Quantitation ◽

Tablet Dosage

A new reverse phase high performance liquid chromatography (RP-HPLC) method has been developed for the simultaneous estimation of gemcitabine hydrochloride and capecitabine hydrochloride in combined tablet dosage form. An inertsil ODS-3 C-18 column having dimensions of 250×4.6 mm and particle size of 5 µm, with mobile phase containing a mixture of acetonitrile : water : triethyelamine in the ratio of (70 : 28 : 2v/v) was used. The pH of mobile phase was adjusted to 4.0 withortho-phosphoric acid. The flow rate was 1 mL/min and the column effluents were monitored at 260 nm. The retention time for gemcitabine hydrochloride and capecitabine hydrochloride was found to be 2.76 and 2.3 min respectively. The proposed method was validated in terms of linearity, accuracy, precision, limit of detection, limit of quantitation and robustness. The method was found to be linear in the range of 10-50 µg/mL and 4-24 µg/mL for gemcitabine hydrochloride and capecitabine hydrochloride, with regression coefficient r = 0.999 and r = 0.999, respectively.

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Box-Behnken Assisted Validation and Optimization of an RP-HPLC Method for Simultaneous Determination of Domperidone and Lansoprazole

Separations ◽

10.3390/separations8010005 ◽

2021 ◽

Vol 8 (1) ◽

pp. 5

Author(s):

Mohd Afzal ◽

Mohd. Muddassir ◽

Abdullah Alarifi ◽

Mohammed Tahir Ansari

Keyword(s):

Flow Rate ◽

Mobile Phase ◽

Limit Of Detection ◽

Hplc Method ◽

Box Behnken Design ◽

Rp Hplc ◽

System Suitability ◽

Method Optimization ◽

Key Variables

A highly specific, accurate, and simple RP-HPLC technique was developed for the real-time quantification of domperidone (DOMP) and lansoprazole (LANS) in commercial formulations. Chromatographic studies were performed using a Luna C8(2), 5 μm, 100Å, column (250 × 4.6 mm, Phenomenex) with a mobile phase composed of acetonitrile/2 mM ammonium acetate (51:49 v/v), pH 6.7. The flow rate was 1 mL·min−1 with UV detection at 289 nm. Linearity was observed within the range of 4–36 µg·mL−1 for domperidone and 2–18 µg·mL−1 for lansoprazole. Method optimization was achieved using Box-Behnken design software, in which three key variables were examined, namely, the flow rate (A), the composition of the mobile phase (B), and the pH (C). The retention time (Y1 and Y3) and the peak area (Y2 and Y4) were taken as the response parameters. We observed that slight alterations in the mobile phase and the flow rate influenced the outcome, whereas the pH exerted no effect. Method validation featured various ICH parameters including linearity, limit of detection (LOD), accuracy, precision, ruggedness, robustness, stability, and system suitability. This method is potentially useful for the analysis of commercial formulations and laboratory preparations.

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