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knowledge and comprehensive survey, metformin, pioglitazone, and glimepiride mixture in dosage form was determined by reversed-phase HPLC (RP-HPLC) [ 3 , 31 – 33 ] but was never determined before by chromatographic techniques in biological samples despite

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Acta Chromatographica
Authors: Muhammad Fawad Rasool, Umbreen Fatima Qureshi, Nazar Muhammad Ranjha, Imran Imran, Mouqadus Un Nisa, and Abdul Majeed

liquid chromatography (RP-HPLC) is the mostly used because of high sensitivity and selectivity and economical [ 19–21 ]. This method was very economical and reliable for the determination and validation of drug in rabbit plasma and pharmaceutical dosage

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. Figure 2. Chromatograms of Klozan® solution Conclusion The newly developed reversed-phase RP-HPLC method was found to be convenient for the simultaneous

Open access
Acta Chromatographica
Authors: A. Suthar, P. Hamarapurkar, P. Patil, M. Phale, K. Katkar, G. Mundada, and V. S. Chauhan

Summary

A simple, specific, and precise RP-HPLC method with photodiode-array detection has been developed for simultaneous analysis of the quinazoline alkaloids vasicine and vasicinone, pharmacologically important constituents of Adhatoda vasica. The compounds were separated by use of 0.1% trifluoroacetic acid in water:acetonitrile 90:10 as isocratic mobile phase at a flow rate of 1.0 mL min−1. Under these conditions, plots of integrated peak area against concentration were linear over the ranges 0.05–10.0 μg mL−1 and 0.5–100.0 μg mL−1 (r 2 = 0.999 and 0.998) for vasicine and vasicinone, respectively. Mean recovery was 99.06% for vasicine and 98.69% for vasicinone. The method is therefore suitable for routine analysis of vasicine and vasicinone in Adhatoda vasica plants of different varieties and in herbal medicinal products prepared from the plants.

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Summary

Methods based on RP-HPLC and HPTLC with UV detection for rapid quantitative determination of marker component in Enicostemma hyssopifolium, swertisin are described. The recovery of the compound was between 96.3–101.5% by HPTLC method and 98.9–100.2% by HPLC assay. The relative standard deviations ranged between 1.53–1.81 (intra-day) and 1.33–1.96 (inter-day) for HPTLC and 0.60–1.11 (intra-day) and 0.80–1.20 (inter-day) for HPLC. The methods were used for routine analysis of swertisin in the aerial parts of the plant. HPTLC method was found to be more economic and less time consuming than HPLC. Reproducibility and recovery in HPLC method were better than that in HPTLC method.

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Linaclotide, a first-in-class guanylate cyclase-C agonist, was recently approved by US Food and Drug Administration (FDA) as a promising pharmacotherapy for the management of constipation-predominant irritable bowel syndrome (IBS). In this communication, we present a novel stability-indicating reverse-phase high-performance liquid chromatography (RP-HPLC) method for the quantitative determination of linaclotide along with its degradation products. During the International Conference on Harmonization (ICH) prescribed stress study, linaclotide was found susceptible to degrade under hydrolytic (acid and base) and oxidative (peroxide) conditions. The separation of the degradants from the analyte was achieved on a Zorbax Eclipse XDB C8 Column (250 mm × 4.6 mm, 5 μm) using 0.01 N potassium dihydrogen orthophosphate buffer and acetonitrile (80:20 v/v) as mobile phase at a flow rate of 1.00 mL min−1 at column temperature of 40 °C. The detection of the column effluents was realized on a photodiode array detector set at 220 nm. Under the above optimal condition, the method was validated with respect to specificity, linearity, range, precision, robustness, and sensitivity in compliance to the regulatory requirements.

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Summary

Ashwaghanda, Withania somnifera, is one of the most widely used herbs in Ayurvedic medicine. Leaves and roots are the traditionally used parts of the plant. An RP-HPLC method using a binary acetonitrile-water gradient containing 0.1% acetic acid has been developed for analysis of withaferin A. The method was validated in accordance with ICH guidelines and used for analysis of the withanolide content of the flowers, leaves, and roots of W. somnifera. The withanolide content was highest in the flowers.

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An effective, reliable, and sensitive reversed-phase high-performance liquid chromatography (RP-HPLC) with diode array detector (DAD) method was investigated for simultaneous determination of polydatin, isoquercitrin, resveratrol, and nicotiflorin in Tetrastigma hemsleyanum. The chromatographic separation of the four compounds was carried out on a Welchrom ODS column (4.6 mm × 250 mm, 5 μm) by gradient elution with phosphoric acid (H3PO4) aqueous solution (0.4%)–methanol as the mobile phase, at the temperature of 30 °C and a flow rate of 1.0 mL/min. The detection wavelength was set at 270 nm. Under optimum conditions, the baseline separation of these four compounds can be performed within 30 min. The developed method was validated in terms of detection limit, quantification limit, linearity, precision, and recovery tests. Eventually, the established HPLC–DAD method was successfully applied to the simultaneous determination of polydatin, isoquercitrin, resveratrol, and nicotiflorin in the extract of herb T. hemsleyanum.

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Summary

Torsemide (TSM) is a loop diuretic used in the treatment of edema, and spironolactone (SPL) is a potassium-sparing diuretic used in hypokalemia. Both are potential diuretics used in combination to treat congestive heart failure. This paper describes a simple, sensitive, accurate, and validated reverse-phase high-performance liquid chromatographic (RP-HPLC) method for the simultaneous quantification of these compounds as the bulk drug and in tablet dosage forms. Separation was carried out on Jasco HPLC system equipped with Neosphere C8 column (150 × 4.6 mm i.d.) and UV/VIS detector using acetonitrile:10 mM potassium dihydrogen phosphate buffer in ratio of 60:40 (υ/υ) as the mobile phase, and detection was carried out at 240 nm. Results were linear in the range of 2–12 μg mL−1 for TSM and 5–30 μg mL−1 for SPL. The method was successfully applied for the analysis of drugs in pharmaceutical formulation. Results of the analysis were validated statistically and by recovery studies.

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Summary

A reverse-phase high-performance liquid chromatographic (RP-HPLC) method was developed for the simultaneous estimation of amlodipine besylate (AMB), valsartan (VAL), and hydrochlorothiazide (HCT) in pharmaceutical formulation using RP-C18 column. The mobile phase (acetonitrile:methanol:50 mM phosphate buffer adjusted to pH 3 with orthophosphoric acid) was pumped at a flow rate of 1.0 mL min−1 in the ratio of 20:50:30% v/v and the eluents were monitored at 239 nm. Linearity was obtained in the concentration range of 0.5–5 μg mL−1 for AMB, 4–40 μg mL−1 for VAL, and 1–10 μg mL−1 for HCT. The method was validated as per International Conference on Harmonization (ICH) guidelines and statistically. The method was validated for accuracy and precision. For precision, the coefficient of variance (COV) was found to be 0.3794, 0.1703 and 0.0578, and for accuracy, it was found to be 0.6351, 0.7688 and 1.1305 for AMB, VAL, and HCT, respectively. The COV values for all the drugs were found to be less than 2%, indicating high degree of precision and accuracy of the proposed high-performance liquid chromatographic (HPLC) method. Owing to its simplicity, rapidness, high precision and accuracy, the proposed HPLC method can be applied for determining AMB, VAL, and HCT in bulk and in pharmaceutical dosage form.

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