Rm Singh

Development and Validation of a RP-HPLC Method for Estimation of Montelukast Sodium in Bulk and in Tablet Dosage Form.

The present work describes a simple, precise and accurate HPLC method for estimation of montelukast sodium in bulk and in tablet dosage form. The separation was achieved by using octadecylsilane column (C18) and acetonitrile:1 mM sodium acetate adjusted to pH 6.3 with acetic acid in proportion of 90:10 v/v as mobile phase, at a flow rate of 1.5 ml/min. Detection was carried out at 285 nm. The retention time of montelukast sodium was found to be 3.4 min. The limit of detection was found 1.31 µg/ml and limit of quantification 3.97 µg/ml. The accuracy and reliability of the proposed method was ascertained by evaluating various validation parameters like linearity (1-100 µg/ml), precision, accuracy and specificity according to ICH guidelines. The proposed method provides an accurate and precise quality control tool for routine analysis of montelukast sodium in bulk and in tablet dosage form.

A simple and sensitive HPTLC method for simultaneous analysis of domperidone and paracetamol in tablet dosage forms

A simple, precise, rapid, selective, and economic high-performance thin-layer chromatographic (HPTLC) method has been established for simultaneous analysis of domperidone (DMP) and paracetamol (PAR) in tablet dosage forms. The chromatographic separation was performed on precoated silica gel 60 GF254 plates with acetone- toluene-methanol 4:4:2 (v/v) as mobile phase. The plates were developed to a distance of 8.0 cm at ambient temperature. The developed plates were scanned and quantified at their single wavelength of maximum absorption at approximately 285 and 248 nm for dom-peridone and paracetamol, respectively. Experimental conditions such as band size, chamber saturation time, migration of solvent front, slit width, etc. were critically studied and the optimum conditions were selected. The drugs were satisfactorily resolved with RF 0.52 ± 0.02 for domperidone and 0.74 ± 0.02 for paracetamol. The method was validated for linearity, accuracy, precision, and specificity. The calibration plot was linear between 16–48 ng per band for DMP and 800-2400 ng per band for PAR. The limits of detection and quantification for DMP were 0.022 and 0.186 ng per band, respectively; for PAR they were 0.307 and 0.931 ng per band. This HPTLC procedure is economic, sensitive, and less time consuming than other chromatographic procedures. It is a user-friendly and important tool for analysis of combined tablet dosage forms.

3-Acetyl-11-keto-β-boswellic acid loaded-polymeric nanomicelles for topical anti-inflammatory and anti-arthritic activity

Objectives The aim of this study was to develop 3‐acetyl‐11‐keto‐β‐boswellic acid (AKBA)‐loaded polymeric nanomicelles for topical anti‐inflammatory and anti‐arthritic activity.

Development and Validation of a RP-HPLC Method for Estimation of Prulifloxacin in Tablet Dosage Form

A simple, precise, rapid, accurate and economic reverse phase high performance liquid chromatographic method has been developed for the estimation of prulifloxacin in tablet dosage form. The separation was achieved by using octadecylsilane column (C18) and KH2PO4 buffer: acetonitrile adjusted to pH 7.3 with triethyl amine in proportion of 10:90 v/v as mobile phase, at a flow rate of 1.0 ml/min. The detection was carried out at 278 nm. The retention time of prulifloxacin was found to be 2.4 min. The limit of detection and limit of quantitation were found to be 0.14 μg/ml and 0.42 μg/ml respectively. The accuracy and reliability of the proposed method was ascertained by evaluating various validation parameters like linearity, precision, accuracy and specificity according to ICH guidelines. The proposed method provides an accurate and precise quality control tool for routine analysis of prulifloxacin in tablet dosage form.

A simple and sensitive HPTLC method for quantitative analysis of artemether and lumefantrine in tablets

A simple, sensitive, precise, rapid, and reliable HPTLC method for quantitative analysis of artemether and lumefantrine in tablets has been established and validated. The method uses aluminum foil plates precoated with silica gel 60 F254 as the stationary phase and nhexaneethyl acetate 8:2 (v/v) as mobile phase. Bands were scanned at 357 nm, the wavelength of maximum absorption. The method is linear (r2 > 0.995), precise (RSD < 2%), accurate (average recovery of 100.5% for artemether and 99.5% for lumefantrine), specific, and robust. The artemether content of the tablets varied from 98.50 to 102.45% and that of lumefantrine from 97.80 to 100.64%. The limits of detection and quantification for artemether were 50 and 150 ng per band, respectively, and those for lumefantrine were 300 and 900 ng per band, respectively. The suitability of this HPTLC method for quantitative analysis of artemether and lumefantrine was proved by validation in accordance with the requirements of pharmaceutical regulatory standards. The method was successfully applied to the analysis of a commercial pharmaceutical tablet dosage form. The method is simple, rapid, reproducible, and accurate and is a more effective option than other chromatographic techniques used for routine quality control.

Development and Validation of a RP-Ultra performance liquid chromatographic Method for Quantification of Topotecan Hydrochloride in Bulk and Injection Dosage Form.

A simple, very fast, precise and accurate reverse phase ultra performance liquid chromatographic method was developed for the determination and validation of topotecan hydrochloride in bulk and injection dosage form. A Waters BEH C18, 50×2.1 mm, 1.7 μm particle size column in gradient mode was used with mobile phase comprising of 0.1% v/v orthophosphoric acid in water and acetonitrile. The analytical column was thermostated at 50° and flow rate was set at 0.4 ml per min, with photo diode array detection at 260 nm. The retention time of topotecan was found 1.38 min. The method was validated in terms of linearity, accuracy, precision and specificity. The calibration curve was found linear between 20 to 60 μg/ml. The limit of detection and limit of quantification were found 0.2353 and 0.7131 μg/ml, respectively. Percentage recoveries were obtained in the range of 98.91% and 99.17%. The proposed method is precise, accurate, selective and reproducible. The ultra performance liquid chromatographic assay procedure, which proved superior because of its greater sensitivity and relatively shorter (4 min) run time, should be an important tool for speedy future analysis of topotecan hydrochloride in bulk and its injection dosage form.

Interactions of herbal extract combinations against free radical scavenging activity

Herbal medicines are often combinations of herbal extracts that are assumed to have additive or synergistic effects. This investigation compared the effect of individual herbal extracts with combinations of extracts on antioxidant activity by 1,1-diphenyl picryl hydrazyl (DPPH) method and showed the additive or synergistic effects by studying interactions between herbal extracts in combination. Curcuma longa Linn. (Zingiberaceae), Bacopa monneira Linn. Penn. (Scrophulariaceae), Zingiber officinale Rosc. (Zingiberaceae) and Emblica officinalis Gaertn. (Euphorbiaceae) were collected and used to prepare the extracts. Effects of the extracts on DPPH scavenging activity were estimated quantitatively by a UV-spectrophotometeric method. Combinations of two herbal extracts of the four active extracts and their interactions were tested by the DPPH method. Each extract significantly scavenges the free radical activity in a dose-dependent manner. The active extracts of Curcuma longa, Bacopa monneira, Zingiber officinale and Emblica officinalis were tested as two-extract combinations. Curcuma longa and Bacopa monneiera, when combined, showed additive effect with a trend towards synergistic effect, whereas Curcuma longa and Emblica officinalis together were additive. The four extracts together were significantly (p ≤ 0.01) more effective than the two-by-two combinations and the individual extracts alone. The less predictable nature of the two-way combinations suggests a need for careful characterization of the effects of each individual herb based on their intended use.

Quality by design approach for simultaneous estimation of doxycycline hyclate and curcumin by RP-HPLC method

A simple, rapid, reliable, robust and optimized reversed phase high performance liquid chromatographic method for simultaneous estimation of doxycycline hyclate and curcumin was successfully developed and validated as per International Conference on Harmonization guidelines. The objective was achieved in terms of well separated peaks within 10 min on a Waters Sunfire C8 column with dimensions of 250×4.6 mm, particle size 5.0 μm using mobile phase consisting of 30 volumes of potassium dihydrogen phosphate buffer (50 mM) adjusted to pH 6.5±0.1 with triethylamine and 70 volumes of methanol at flow rate of 0.85 ml/min. The column effluents were monitored at 400 nm maintained at ambient column temperature (28o). The developed method was found linear over the concentration range of 200-700 μg/ml for doxycycline hyclate and 8-28 μg/ml for curcumin, the detection and quantitation limit was found to be 26.063 and 78.97 μg/ml for doxycycline hyclate; 0.795 and 2.13 μg/ml for curcumin, respectively. The developed method was optimized using Minitab software version 16 to meet the current quality by design requirements. The method validation was done for linearity, range, detection and quantitation limit, accuracy, precision, specificity, system suitability testing, and robustness.