Scientia Pharmaceutica

410 KiB

Open AccessReview

Pharmacological and Phytochemical Appraisal of Selected Medicinal Plants from Jordan with Claimed Antidiabetic Activities

by Fatma U. AFIFI and Violet KASABRI

Sci. Pharm. 2013, 81(4), 889-932; https://doi.org/10.3797/scipharm.1212-20 - 15 Oct 2013

Cited by 28 | Viewed by 2707

Abstract

Plant species have long been regarded as possessing the principal ingredients used in widely disseminated ethnomedical practices. Different surveys showed that medicinal plant species used by the inhabitants of Jordan for the traditional treatment of diabetes are inadequately screened for their therapeutic/preventive potential [...] Read more.

Plant species have long been regarded as possessing the principal ingredients used in widely disseminated ethnomedical practices. Different surveys showed that medicinal plant species used by the inhabitants of Jordan for the traditional treatment of diabetes are inadequately screened for their therapeutic/preventive potential and phytochemical findings. In this review, traditional herbal medicine pursued indigenously with its methods of preparation and its active constituents are listed. Studies of random screening for selective antidiabetic bioactivity and plausible mechanisms of action of local species, domesticated greens, or wild plants are briefly discussed. Recommended future directives incurring the design and conduct of comprehensive trials are pointed out to validate the usefulness of these active plants or bioactive secondary metabolites either alone or in combination with existing conventional therapies. Full article

513 KiB

Open AccessArticle

Erratum to "Intranasal Delivery of Chitosan Nanoparticles for Migraine Therapy" [Sci Pharm. 2013; 81: 843–854]

by Neha GULATI, Upendra NAGAICH and Shubhini A. SARAF

Sci. Pharm. 2013, 81(4), 1167-1172; https://doi.org/10.3797/scipharm.1208-18err - 6 Oct 2013

Cited by 1 | Viewed by 2388

Abstract

This is an erratum to the article 'Intranasal Delivery of Chitosan Nanoparticles for Migraine Therapy' [Sci Pharm. 2013; 81: 843–854]. Figures 1–3 are added. Full article

361 KiB

Open AccessArticle

Design of Experiment (DOE) Utilization to Develop a Simple and Robust Reversed-Phase HPLC Technique for Related Substances’ Estimation of Omeprazole Formulations

by Vayeda Chintan MANRANJAN, Devendra Singh YADAV, Hitesh Amrutlal JOGIA and Praful Lalitkumar CHAUHAN

Sci. Pharm. 2013, 81(4), 1043-1056; https://doi.org/10.3797/scipharm.1306-06 - 12 Aug 2013

Cited by 13 | Viewed by 2136

Abstract

A simple, fast, and sensitive reversed-phase HPLC method with UV detection was developed for the quantitation of omeprazole and its eleven related compounds (impurities) in pharmaceutical formulation using the Thermo Accucore C–18 (50 mm x 4.6 mm, 2.6 μm) column. The separation among [...] Read more.

A simple, fast, and sensitive reversed-phase HPLC method with UV detection was developed for the quantitation of omeprazole and its eleven related compounds (impurities) in pharmaceutical formulation using the Thermo Accucore C–18 (50 mm x 4.6 mm, 2.6 μm) column. The separation among all the compounds was achieved with a flow rate of 0.8 mL min⁻¹ employing a gradient program of mobile phase A [0.08 M glycine buffer pH 9.0: acetonitrile; 95:05 (v/v)] and mobile phase B [acetonitrile: methanol; 65:35 (v/v)]. The chromatographic detection was carried out at a wavelength of 305 nm. The method was validated for specificity, linearity, and recovery. The huskiness of the method was determined prior to validation using the Design of Experiments (DOE). The ANOVA analysis of DOE with a 95% confidence interval (CI) confirmed the buffer pH of mobile phase A (p <0.0001) and column temperature (p<0.0001) as significant Critical Method Parameters (CMPs). Full article

273 KiB

Open AccessArticle

Determination of Cephalexin Monohydrate in Pharmaceutical Dosage Form by Stability-Indicating RP-UFLC and UV Spectroscopic Methods

by Sagar Suman PANDA, Bera V. V. RAVI KUMAR, Rabisankar DASH and Ganeswar MOHANTA

Sci. Pharm. 2013, 81(4), 1029-1042; https://doi.org/10.3797/scipharm.1306-07 - 31 Jul 2013

Cited by 24 | Viewed by 2314

Abstract

An ultra-fast liquid chromatographic method and two UV spectroscopic methods were developed for the determination of cephalexin monohydrate in pharmaceutical dosage forms. Isocratic separation was performed on an Enable C₁₈G column (250 mm × 4.6 mm i.d., 5 μm) using methanol:0.01 [...] Read more.

An ultra-fast liquid chromatographic method and two UV spectroscopic methods were developed for the determination of cephalexin monohydrate in pharmaceutical dosage forms. Isocratic separation was performed on an Enable C₁₈G column (250 mm × 4.6 mm i.d., 5 μm) using methanol:0.01 M TBAHS (50:50, v/v) as the mobile phase at a flow rate of 1.0 ml/min. The PDA detection wavelength was set at 254 nm. The UV spectroscopic method was performed at 261 nm and at 256-266 nm for the AUC method using a phosphate buffer (pH=5.5). The linearity was observed over a concentration range of 1.0–120 μg/ml for UFLC and both of the UV spectroscopic methods (correlation coefficient=0.999). The developed methods were validated according to ICH guidelines. The relative standard deviation values for the intraday and interday precision studies were < 2%, and the accuracy was > 99% for all of the three methods. The developed methods were used successfully for the determination of cephalexin in dry syrup formulation. Full article

450 KiB

Open AccessArticle

Effect of Tephrosia purpurea (L.) Pers. Leaves on Gentamicin-Induced Nephrotoxicity in Rats

by Avijeet JAIN, Alok NAHATA and Abhay Kumar SINGHAI

Sci. Pharm. 2013, 81(4), 1071-1088; https://doi.org/10.3797/scipharm.1302-09 - 22 Jul 2013

Cited by 10 | Viewed by 1648

Abstract

The aim of the study was to evaluate the nephroprotective and nephrocurative effects of Tephrosia purpurea (L.) Pers. leaves against gentamicin-induced acute renal injury in albino rats. The maximum free radical scavenging activity of the ethanolic extract was the basis for the selection [...] Read more.

The aim of the study was to evaluate the nephroprotective and nephrocurative effects of Tephrosia purpurea (L.) Pers. leaves against gentamicin-induced acute renal injury in albino rats. The maximum free radical scavenging activity of the ethanolic extract was the basis for the selection of this extract for the in vivo study. Gentamicin (40 mg/kg, s.c.) was administered to induce toxicity in the toxic group and the ethanolic extract (200 mg/kg p.o.) was administered in all treated groups. Blood urea and serum creatinine levels were monitored to assess the effects. The antioxidant potential was also evaluated by the estimation of reduced glutathione (GSH) and malondialdehyde (MDA). Gentamicin intoxication caused significant increases in blood urea and serum creatinine levels as compared to the normal control. In the preventive regimen, the extract (200 mg/kg, p.o.) showed significant reductions in the elevated blood urea and serum creatinine. Histopathological changes were in accordance with the biochemical findings. Also in the curative regimen, the blood urea and serum creatinine levels revealed significant curative effects. In our in vivo antioxidant activity, the GSH level was significantly (P< 0.05) increased in the extract-treated groups, whereas MDA was reduced significantly (P< 0.05). Further thin layer chromatography (TLC) and high-performance thin layer chromatography (HPTLC) led us to ascertain the presence of rutin and quercetin in the extract. We were able to isolate and characterize an isolate from the ethanolic extract and characterize it on the basis of chromatographic, melting point, FTIR, NMR, and mass spectroscopic studies. The findings suggest that the ethanol extract of Tephrosia purpurea leaves possesses marked nephroprotective and curative activities without any toxicity. The proposed mechanisms for the claimed activity are antioxidant activity and the inhibition of an overproduction of NO and Cox-2 expression. These activities may be attributed to the presence of phenolics and flavonoidal compounds like rutin and quercetin. Thus, it can be said that Tephrosia purpurea could offer a promising role in the treatment of acute renal injury caused by nephrotoxins like gentamicin. Full article

219 KiB

Open AccessArticle

Development and Validation of a Stability-Indicating Assay of Etofenamate by RP-HPLC and Characterization of Degradation Products

by Ramalingam PERAMAN, Devanna NAYAKANTI, Hari Hara THEJA DUGGA and Sudhakara KODIKONDA

Sci. Pharm. 2013, 81(4), 1017-1028; https://doi.org/10.3797/scipharm.1305-19 - 22 Jul 2013

Cited by 8 | Viewed by 1784

Abstract

A validated stability-indicating RP-HPLC method for etofenamate (ETF) was developed by separating its degradation products on a C18 (250 mm × 4.6 mm 5 μm) Qualisil BDS column using a phosphate buffer (pH-adjusted to 6.0 with orthophosphoric acid) and methanol in the ratio [...] Read more.

A validated stability-indicating RP-HPLC method for etofenamate (ETF) was developed by separating its degradation products on a C18 (250 mm × 4.6 mm 5 μm) Qualisil BDS column using a phosphate buffer (pH-adjusted to 6.0 with orthophosphoric acid) and methanol in the ratio of 20:80 % v/v as the mobile phase at a flow rate of 1.0 mL/min. The column effluents were monitored by a photodiode array detector set at 286 nm. The method was validated in terms of specificity, linearity, accuracy, precision, detection limit, quantification limit, and robustness. Forced degradation of etofenamate was carried out under acidic, basic, thermal, photo, and peroxide conditions and the major degradation products of acidic and basic degradation were isolated and characterized by 1H-NMR, 13C-NMR, and mass spectral studies. The mass balance of the method varied between 92–99%. Full article

261 KiB

Open AccessArticle

Liposomes for Topical Use: A Physico-Chemical Comparison of Vesicles Prepared from Egg or Soy Lecithin

by Lívia BUDAI, Nóra KASZÁS, Pál GRÓF, Katalin LENTI, Katayoon MAGHAMI, István ANTAL, Imre KLEBOVICH, Ilona PETRIKOVICS and Marianna BUDAI

Sci. Pharm. 2013, 81(4), 1151-1166; https://doi.org/10.3797/scipharm.1305-11 - 14 Jul 2013

Cited by 35 | Viewed by 3024

Abstract

Developments in nanotechnology and in the formulation of liposomal systems provide the opportunity for cosmetic dermatology to design novel delivery systems. Determination of their physico-chemical parameters has importance when developing a nano-delivery system. The present study highlights some technological aspects/characteristics of liposomes formulated [...] Read more.

Developments in nanotechnology and in the formulation of liposomal systems provide the opportunity for cosmetic dermatology to design novel delivery systems. Determination of their physico-chemical parameters has importance when developing a nano-delivery system. The present study highlights some technological aspects/characteristics of liposomes formulated from egg or soy lecithins for topical use. Alterations in the pH, viscosity, surface tension, and microscopic/macroscopic appearance of these vesicular systems were investigated. The chemical composition of the two types of lecithin was checked by mass spectrometry. Caffeine, as a model molecule, was encapsulated into multilamellar vesicles prepared from the two types of lecithin: then zeta potential, membrane fluidity, and encapsulation efficiency were compared. According to our observations, samples prepared from the two lecithins altered the pH in opposite directions: egg lecithin increased it while soy lecithin decreased it with increased lipid concentration. Our EPR spectroscopic results showed that the binding of caffeine did not change the membrane fluidity in the temperature range of possible topical use (measured between 2 and 50 °C). Combining our results on encapsulation efficiency for caffeine (about 30% for both lecithins) with those on membrane fluidity data, we concluded that the interaction of caffeine with the liposomal membrane does not change the rotational motion of the lipid molecules close to the head group region. In conclusion, topical use of egg lecithin for liposomal formulations can be preferred if there are no differences in the physico-chemical properties due to the encapsulated drugs, because the physiological effects of egg lecithin vesicles on skin are significantly better than that of soy lecithin liposomes. Full article

755 KiB

Open AccessArticle

Ascorbic Acid for the Safe Use of a Sunscreen Agent: Accumulation of Nano Zinc Oxide and Titanium Dioxide on the Skin

by Anahita FATHI-AZARBAYJANI, Poh Leng TAN, Yew Ying CHAN and Sui Yung CHAN

Sci. Pharm. 2013, 81(4), 1141-1150; https://doi.org/10.3797/scipharm.1306-05 - 14 Jul 2013

Cited by 13 | Viewed by 2463

Abstract

Objective: Physical UV absorbers such as titanium dioxide or zinc oxide have been found to be highly protective against ultraviolet radiation. Sun protection factor depends on the accumulation of the minerals on the skin. UV-absorbing agents must accumulate within the upper skin layers [...] Read more.

Objective: Physical UV absorbers such as titanium dioxide or zinc oxide have been found to be highly protective against ultraviolet radiation. Sun protection factor depends on the accumulation of the minerals on the skin. UV-absorbing agents must accumulate within the upper skin layers in order to provide a dense light-absorbing layer and guarantee water resistance. The aim of this work was to increase the skin deposition and efficacy of sunscreens without increasing their skin permeation. The application possibility of EDX to determine the quantitative elemental composition of zinc and titanium on the skin surface was studied. Method: The changes induced in the skin deposition of physical UV absorbers in conjunction with ascorbic acid were studied. In vitro skin permeation and X-ray elemental analysis were carried out to determine the mineral skin deposition effect of ascorbic acid. Key findings: Results indicate that ascorbic acid may significantly increase the skin deposition (p < 0.05) of these minerals on the skin without increasing their skin permeation (p > 0.05). Flow through diffusion cell and X-ray elemental analyses appear to be complementary and show that ascorbic acid is able to increase accumulation of sunscreen on the skin. Full article

1327 KiB

Open AccessArticle

Stability-Indicating UPLC Method for Tramadol HCl Impurities in the Tramadol Injection after Dilution by Infusion Fluids (5% Dextrose and 0.9% Sodium Chloride)

by Anil K. BINNOR, Khagga MUKKANTI, Mulukutla V. SURYANARAYANA and Sunilendu B. ROY

Sci. Pharm. 2013, 81(4), 1003-1016; https://doi.org/10.3797/scipharm.1305-20 - 14 Jul 2013

Cited by 4 | Viewed by 1671

Abstract

A novel, rapid, and sensitive ultra-performance liquid chromatography (UPLC) method has been developed and validated as per ICH guidelines for the determination of tramadol HCl impurities in the tramadol HCl injection after reconstitution by infusion fluids (5% dextrose and 0.9% sodium chloride). The [...] Read more.

A novel, rapid, and sensitive ultra-performance liquid chromatography (UPLC) method has been developed and validated as per ICH guidelines for the determination of tramadol HCl impurities in the tramadol HCl injection after reconstitution by infusion fluids (5% dextrose and 0.9% sodium chloride). The tramadol HCl injection is for the treatment of patients with moderate-to-severe pain. The stability of the reconstituted solution is critical before intravenous injection. The literature search resulted in few published articles on assays of tramadol in infusion fluids by conventional HPLC. No attempts have yet been made to determine the impurities in infusion fluids, as the concentration of tramadol after reconstitution is extremely low (0.4 mg/mL) and that of impurities is even lower. The proposed method is novel as it allows the quantitation of the impurities of tramadol HCl and is based on modern chromatographic techniques like UPLC. The method was developed using the Waters Acquity BEH C18 column with a mobile phase consisting of a gradient mixture of solvent A (trifluroacetic acid buffer) and solvent B (methanol: acetonitrile). The model stability study was designed by diluting the tramadol HCl injection in the 5% dextrose injection and 0.9% sodium chloride injection. Each mixture was kept under storage at room temperature (25 ± 2°C) for testing at initial, 2, 4, 8, 12, 18 & 24 hours. The validation study illustrates that the proposed method is suitable for the determination of tramadol and its impurities. The proposed method makes use of the LC-MS-compatible mobile phase. It can be useful for the determination of tramadol HCl and its impurities in plasma samples and other pharmaceutical dosage forms. Full article

363 KiB

Open AccessArticle

Chemometrics-Assisted UV Spectrophotometric and RP-HPLC Methods for the Simultaneous Determination of Tolperisone Hydrochloride and Diclofenac Sodium in their Combined Pharmaceutical Formulation

by Nikunj Rameshbhai GOHEL, Bhavin Kiritbhai PATEL and Vijaykumar Kunvarji PARMAR

Sci. Pharm. 2013, 81(4), 983-1002; https://doi.org/10.3797/scipharm.1306-01 - 14 Jul 2013

Cited by 4 | Viewed by 2154

Abstract

Chemometrics-assisted UV spectrophotometric and RP-HPLC methods are presented for the simultaneous determination of tolperisone hydrochloride (TOL) and diclofenac sodium (DIC) from their combined pharmaceutical dosage form. Chemometric methods are based on principal component regression and partial least-square regression models. Two sets of standard [...] Read more.

Chemometrics-assisted UV spectrophotometric and RP-HPLC methods are presented for the simultaneous determination of tolperisone hydrochloride (TOL) and diclofenac sodium (DIC) from their combined pharmaceutical dosage form. Chemometric methods are based on principal component regression and partial least-square regression models. Two sets of standard mixtures, calibration sets, and validation sets were prepared. Both models were optimized to quantify each drug in the mixture using the information included in the UV absorption spectra of the appropriate solution in the range 241–290 nm with the intervals λ = 1 nm at 50 wavelengths. The optimized models were successfully applied to the simultaneous determination of these drugs in synthetic mixture and pharmaceutical formulation. In addition, an HPLC method was developed using a reversed-phase C18 column at ambient temperature with a mobile phase consisting of methanol:acetonitrile:water (60:30:10 v/v/v), pH-adjusted to 3.0, with UV detection at 275 nm. The methods were validated in terms of linearity, accuracy, precision, sensitivity, specificity, and robustness in the range of 3–30 μg/mL for TOL and 1–10 μg/mL for DIC. The robustness of the HPLC method was tested using an experimental design approach. The developed HPLC method, and the PCR and PLS models were used to determine the amount of TOL and DIC in tablets. The data obtained from the PCR and PLS models were not significantly different from those obtained from the HPLC method at 95% confidence limit. Full article

410 KiB

Open AccessArticle

Stability-Indicating RP-HPLC Method for the Simultaneous Estimation of Doxofylline and Terbutalinesulphate in Pharmaceutical Formulations

by Gananadhamu SAMANTHULA, Krishnaveni YADIKI, Shantikumar SALADI, Sreekanth GUTALA and K. V. SURENDRANATH

Sci. Pharm. 2013, 81(4), 969-982; https://doi.org/10.3797/scipharm.1305-14 - 14 Jul 2013

Cited by 7 | Viewed by 1795

Abstract

An isocratic, stability-indicating, reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed for the quantitative determination of doxofylline and terbutaline sulphate, used for the treatment of respiratory problems. The chromatographic separation was achieved on a Zorbax-SB Phenyl 250 x 4.6mm x 5 μm column [...] Read more.

An isocratic, stability-indicating, reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed for the quantitative determination of doxofylline and terbutaline sulphate, used for the treatment of respiratory problems. The chromatographic separation was achieved on a Zorbax-SB Phenyl 250 x 4.6mm x 5 μm column with the mobile phase consisting of a mixture of 25 mM ammonium acetate (pH 5.0) : acetonitrile (85:15 %v/v) at a flow rate of 1.0 ml/min. The eluate was monitored at 274 nm using a PDA detector. Forced degradation studies were performed on the bulk sample of doxofylline and terbutaline sulphate using acid (0.1N HCl), base (0.1N NaOH), oxidation (10% hydrogen peroxide), photolytic, and thermal degradation conditions. Good resolution was observed between the degradants and analytes. Degradation products resulting from the stress studies did not interfere with the detection of doxofylline and terbutaline sulphate, thus the assay is stability-indicating. The method has the requisite accuracy, selectivity, sensitivity, and precision for the simultaneous estimation of doxofylline and terbutaline sulphate in bulk and pharmaceutical dosage forms. The limit of quantitation and limit of detection were found to be 1.16 μg/ml and 0.38 μg/ml for doxofylline, 2.08 μg/ml and 0.62 μg/ml for terbutaline sulphate, respectively. Full article

330 KiB

Open AccessArticle

Comparison Study of Oral Iron Preparations Using a Human Intestinal Model

by Mohammed Gulrez ZARIWALA, Satyanarayana SOMAVARAPU, Sebastien FARNAUD and Derek RENSHAW

Sci. Pharm. 2013, 81(4), 1123-1140; https://doi.org/10.3797/scipharm.1304-03 - 21 Jun 2013

Cited by 39 | Viewed by 4347

Abstract

Iron deficiency and related iron deficiency anaemia (IDA) are the most prevalent nutritional disorders worldwide. The standard treatment involves supple-mentation with solid or liquid iron supplement preparations, usually based on a ferrous salt such as ferrous sulphate, ferrous fumarate, or ferrous gluconate. In [...] Read more.

Iron deficiency and related iron deficiency anaemia (IDA) are the most prevalent nutritional disorders worldwide. The standard treatment involves supple-mentation with solid or liquid iron supplement preparations, usually based on a ferrous salt such as ferrous sulphate, ferrous fumarate, or ferrous gluconate. In the present study, we compared iron uptake and absorption from various solid and liquid iron supplement preparations currently available in the United Kingdom using the well-characterised human epithelial adenocarcinoma cell line Caco-2. Intracellular ferritin protein formation by the Caco-2 cell was con-sidered an indicator of cellular iron uptake and absorption. We investigated the effects of formulation ingredients at a defined pH on iron uptake and absorption, and designed a novel two-stage dissolution-absorption protocol that mimicked physiological conditions. Our experiments revealed wide variations in the rate of dissolution between the various solid iron preparations. Conventional-release ferrous iron tablets dissolved rapidly (48 ± 4 mins to 64 ± 4 mins), whereas modified-released tablets and capsules took significantly longer to undergo complete dissolution (274 ± 8 to 256 ± 8 mins). Among the solid iron prepa-rations, ferrous sulphate conventional-release tablets demonstrated the highest iron absorption, whereas modified-release ferrous preparations demonstrated uniformly low iron absorption, as compared to the control (P < 0.05). Taken together, our results demonstrate that there are wide-ranging variations in dissolution times and iron uptake from oral iron preparations, with the physical characteristics of the preparation as well as the form of iron playing a key role. Full article

230 KiB

Open AccessArticle

Ant Plant (Myrmecodia tuberosa) Hypocotyl Extract Modulates TCD4+ and TCD8+ Cell Profile of Doxorubicin-Induced Immune-Suppressed Sprague Dawley Rats In Vivo

by SUMARDI, Triana HERTIANI and Ediati SASMITO

Sci. Pharm. 2013, 81(4), 1057-1070; https://doi.org/10.3797/scipharm.1302-03 - 21 Jun 2013

Cited by 16 | Viewed by 2046

Abstract

Myrmecodia tuberosa Jack (Rubiaceae) has been used as part of traditional Indonesian remedies for a wide range of therapeutic usages in West Papua. Our preliminary study revealed the significant potency of these plant extracts and fractions as an immunomodulator by an in vitro [...] Read more.

Myrmecodia tuberosa Jack (Rubiaceae) has been used as part of traditional Indonesian remedies for a wide range of therapeutic usages in West Papua. Our preliminary study revealed the significant potency of these plant extracts and fractions as an immunomodulator by an in vitro technique on Balb/c mice. This study explored the effect of M. tuberosa hypocotyl ethanol extract on the TCD4+ and TCD8+ cell profiles of doxorubicin (Dox)-induced immune-suppressed Sprague Dawley (SD) rats by an in vivo method. Dried powder of M. tuberosa hypocotyl was macerated in 95% ethanol. Following solvent evaporation in a vacuum, the ethanol extract (EE) was partitioned to yield an n-hexane fraction (FH) and residue (FNH). FNH was further partitioned to yield ethyl acetate (FEtOAc) and water fractions (FW). The extract and fractions in the concentrations 10, 20, 50, and 100 μg/mL were tested on macrophage cells by the latex bead method, while the proliferation of lymphocyte cells was evaluated by the MTT assay. The total phenolic and flavonoid contents of those fractions were evaluated. The active fraction was administrated orally on Dox-induced SD rats for 28 days by an in vivo method to observe the TCD4+ and TCD8+ cell profiles. The in vivo assay showed that the FNH could maintain the number of TCD4+ cells, but not the number of TCD8+ cells. The ED50 observed was 24.24 mg/kg BW. Steroid/terpenoid compounds were detected in this fraction along with the phenolics and flavonoids. The FNH contained 3.548 ± 0.058% GAE of total phenolics and 0.656 ± 0.026% QE of total flavonoids. M. tuberosa hypocotyl extract is a potent immunomodulatory agent and may act as co-chemotherapy in Dox use. Full article

219 KiB

Open AccessArticle

Development and Validation of a Stability-Indicating RP-HPLC Method for the Simultaneous Determination of Phenoxyethanol, Methylparaben, Propylparaben, Mometasone Furoate, and Tazarotene in Topical Pharmaceutical Dosage Formulation

by Chinmoy ROY and Jitamanyu CHAKRABARTY

Sci. Pharm. 2013, 81(4), 951-968; https://doi.org/10.3797/scipharm.1303-22 - 4 Jun 2013

Cited by 23 | Viewed by 2848

Abstract

A stability-indicating RP-HPLC method has been developed and validated for the simultaneous determination of phenoxyethanol (PE), methylparaben (MP), propylparaben (PP), mometasone furoate (MF), and tazarotene (TA) in topical pharmaceutical dosage formulation. The desired chromatographic separation was achieved on the Waters X-Bridge^TM C18 [...] Read more.

A stability-indicating RP-HPLC method has been developed and validated for the simultaneous determination of phenoxyethanol (PE), methylparaben (MP), propylparaben (PP), mometasone furoate (MF), and tazarotene (TA) in topical pharmaceutical dosage formulation. The desired chromatographic separation was achieved on the Waters X-Bridge^TM C18 (50×4.6mm, 3.5μ) column using gradient elution at 256 nm detection wavelength. The optimized mobile phase consisted of 0.1%v/v orthophosphoric acid in water as solvent-A and acetonitrile as solvent-B. The method showed linearity over the range of 5.88–61.76 μg/mL, 0.18–62.36 μg/mL, 0.17–6.26 μg/mL, 0.47–31.22 μg/mL, and 0.44–30.45 μg/mL for PE, MP, PP, MF, and TA, respectively. The recovery for all of the components was in the range of 98-102%. The stability-indicating capability of the developed method was established by analysing the forced degradation samples, in which the spectral purity of PE, MP, PP, MF, and TA along with the separation of degradation products from the analyte peaks was achieved. The proposed method was successfully applied for the quantitative determination of PE, MP, PP, MF, and TA in a cream sample. Full article

441 KiB

Open AccessArticle

Isolation and Characterisation of Degradation Impurities in the Cefazolin Sodium Drug Substance

by Balasubramanian SIVAKUMAR, Kannabiran PARTHASARATHY, Raman MURUGAN, Ramajeyabalan JEYASUDHA, Saravanan MURUGAN and Rajendira JANARDHAN SARANGHDAR

Sci. Pharm. 2013, 81(4), 933-950; https://doi.org/10.3797/scipharm.1304-14 - 4 Jun 2013

Cited by 6 | Viewed by 2282

Abstract

Two unknown impurities were detected in the cefazolin sodium bulk drug substance using gradient reversed-phase high-performance liquid chromate-graphy (HPLC). These impurities were isolated by preparative HPLC and characterized by using spectroscopic techniques like LC-MS, LC-MS/MS, 1D, 2D NMR, and FT-IR. Based on the [...] Read more.

Two unknown impurities were detected in the cefazolin sodium bulk drug substance using gradient reversed-phase high-performance liquid chromate-graphy (HPLC). These impurities were isolated by preparative HPLC and characterized by using spectroscopic techniques like LC-MS, LC-MS/MS, 1D, 2D NMR, and FT-IR. Based on the spectral data, the impurities have been characterized as N-(2,2-dihydroxyethyl)-2-(1H-tetrazol-1-yl)acetamide (Impu rity-I) and 2-{carboxy[(1H-tetrazol-1-ylacetyl)amino]methyl}-5-methylidene-5,6-dihydro-2H-1,3-thiazine-4-carboxylic acid (Impurity-II). The structures of these impurities were also established unambiguously by co-injection into HPLC to confirm the retention time. To the best of our knowledge, these two impurities were not reported elsewhere. Full article

1539 KiB

Open AccessArticle

Application of an Amine Functionalized Biopolymer in the Colonic Delivery of Glycyrrhizin: A Design and In Vivo Efficacy Study

by Amit KUMAR DE, Sriparna DATTA and Arup MUKHERJEE

Sci. Pharm. 2013, 81(4), 1101-1122; https://doi.org/10.3797/scipharm.1301-14 - 18 May 2013

Cited by 3 | Viewed by 1888

Abstract

In our current study, a newer amine functionalized guar gum derivative was studied for its efficacy in colonic drug delivery. Glycyrrhizic acid mono-ammonium salt was used as the model drug. Drug-loaded microparticles were formulated by ionic crosslinking using sodium tripolyphosphate. The Scanning Electron [...] Read more.

In our current study, a newer amine functionalized guar gum derivative was studied for its efficacy in colonic drug delivery. Glycyrrhizic acid mono-ammonium salt was used as the model drug. Drug-loaded microparticles were formulated by ionic crosslinking using sodium tripolyphosphate. The Scanning Electron Microscopic study revealed spherical particles of sizes from 4.9 ± 3.8 μm to 6.9 ± 3.9 μm. The FT-IR studies presented a possible interaction between the drug and the polymer. The drug was encapsulated in amorphous form as observed from the powder X-Ray Diffraction studies. A cumulative drug release study was carried out in simulated gastric, intestinal, and colonic fluids. The cumulative drug release studies presented a burst release followed by a sustained release of the drug in simulated colonic fluid containing rat cecal contents. The drug-polymer ratio was optimised using a 3² factorial design by taking the amounts of glycyrrhizic acid (X₁) and guar gum alkyl amine (X₂) as the independant variables. The percent cumulative drug release at 240 mins (Q₂₄₀), 720 mins (Q₇₂₀), and at 1,440 mins (Q₁₄₄₀) were considered as the dependant variables. The efficacy of the optimized formulation was studied in a 2,4,6-trinitrobenzene sulfonic acid-induced rat colitis model. The tissue’s nitric oxide, malondialdehyde, and myeloperoxidase activities were found to be much lower in the microparticle-treated group compared to free drug-treated group. The histology of the colonic tissue from the treated group of animals revealed almost no infiltration of inflammatory cells in the tissue for the microparticle-treated group of animals. The synthesized amine derivative of guar gum was found to be better in vitro with a better in vivo efficacy in the colonic delivery of glycyrrhizic acid monoammonium salt and can be considered as a newer modified biopolymer for colonic drug delivery. Full article

297 KiB

Open AccessArticle

Accelerated Stability Testing of a Clobetasol Propionate-Loaded Nanoemulsion as per ICH Guidelines

by Mohammad Sajid ALI, Mohammad Sarfaraz ALAM, Nawazish ALAM, Tarique ANWER and Mohammed Mohsen A. SAFHI

Sci. Pharm. 2013, 81(4), 1089-1100; https://doi.org/10.3797/scipharm.1210-02 - 7 Apr 2013

Cited by 26 | Viewed by 2883

Abstract

The physical and chemical degradation of drugs may result in altered therapeutic efficacy and even toxic effects. Therefore, the objective of this work was to study the stability of clobetasol propionate (CP) in a nanoemulsion. The nanoemulsion formulation containing CP was prepared by [...] Read more.

The physical and chemical degradation of drugs may result in altered therapeutic efficacy and even toxic effects. Therefore, the objective of this work was to study the stability of clobetasol propionate (CP) in a nanoemulsion. The nanoemulsion formulation containing CP was prepared by the spontaneous emulsification method. For the formulation of the nanoemulsion, Safsol, Tween 20, ethanol, and distilled water were used. The drug was incorporated into an oil phase in 0.05% w/v. The lipophilic nature of the drug led to the O/W nano-emulsion formulation. This was characterized by droplet size, pH, viscosity, conductivity, and refractive index. Stability studies were performed as per ICH guidelines for a period of three months. The shelf life of the nanoemulsion formulation was also determined after performing accelerated stability testing (40°C ± 2°C and 75% ± 5% RH). We also performed an intermediate stability study (30°C ± 2°C / 65% RH ± 5% RH). It was found that the droplet size, conductivity, and refractive index were slightly increased, while the viscosity and pH slightly decreased at all storage conditions during the 3-month period. However, the changes in these parameters were not statistically significant (p≥0.05). The degradation (%) of the optimized nanoemulsion of CP was determined and the shelf life was found to be 2.18 years at room temperature. These studies confirmed that the physical and chemical stability of CP were enhanced in the nanoemulsion formulation. Full article

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Sci. Pharm., Volume 81, Issue 4 (December 2013) – 17 articles , Pages 889-1172

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