Abstract: Olive is grown in semi-arid climatic conditions; however, little is known about mineral changes in olive plant and nutrient requirements during the production period. Hence, the current study was conducted under Pothwar agro-climatic conditions in order to select appropriate stage of macronutrients (N, P, K) application in relation to soil and leaf nutritional status during 2017 and 2018 growing seasons. Soil and leaf analysis were performed at four different phenological stages (i.e. flowering, fruit setting, fruit enlargement and fruit maturity stages). The results revealed that the assessed macronutrient in leaf and soil varied significantly among varieties, phenological stages and growing year. The results revealed also that nitrogen level was found to decrease from fruit set (1.56%) to fruit enlargement stage (1.47%). Leaf and soil N, P and K contents were found higher before the flowering (stage 1) and depleted after fruit harvesting (stage 4), regardless of olive varieties. However, high yielding varieties showed lower nutrients after fruit harvesting (stage 4). Therefore, N content in leaf and soil gradually decreased during fruit growth and development. Whereas, K content in leaf and soil sharply declined from fruit maturity to fruit ripening stage. Overall, the trend of nutrient depletion showed that plants need phosphorus for fruit setting, nitrogen before and after fruit setting, and potash after pit hardening or at oil accumulation stages.

Resumo O padrão de distribuição e a abundância relativa de pragas de roedores agrícolas nas áreas irrigadas e irrigadas do distrito Swat Khyber Pakhtunkhwa, Paquistão foram registrados de abril de 2011 a novembro de 2013 usando armadilhas vivas de malha de arame. Um total de 350 roedores (269 Rattus rattus e 81 Mus musculus) foram capturados em 2268 noites de armadilha (sucesso da armadilha: 0,15). A regressão das capturas diárias em capturas cumulativas revelou uma estimativa de 350 roedores de todas as estruturas amostradas, com uma média de 21,8 roedores por campo agrícola. Os ratos domésticos (R. rattus; 76,8% das capturas) foram numericamente dominantes em quase todos os tipos de campos agrícolas e foram significativamente diferentes dos camundongos (Mus musculus; 23,1% das capturas). Ambas as espécies foram encontradas juntas em alguns campos. A proporção de sexo revelou que os machos superaram as fêmeas em ambas as espécies relatadas.

Abstract Distribution pattern and relative abundance of the agricultural rodent pests of rain-fed and irrigated areas of district Swat Khyber Pakhtunkhwa, Pakistan were recorded from April 2011 to November 2013 using wire mesh live traps. A total of 350 rodents (269 Rattus rattus and 81 Mus musculus) were captured under 2268 trap nights (trap success: 0.15). Regression of daily captures on cumulative captures revealed an estimate of 350 rodents from all the sampled structures with an average of 21.8 rodents per crop field. House rats (R. rattus; 76.8% of captures) were numerically dominant in almost all types of agricultural fields, and were significantly different from the mice (Mus musculus; 23.1% of captures). Both species were found together in some fields. The sex ratio revealed that males outnumbered the females in both of the reported species.

Green synthesis of nanoparticles has received a lot of attention from scientists globally because it is eco-friendly, relatively rapid, and a cost-effective method. This work presents a method for the green synthesis of nickel oxide nanoparticles (NiO-NPs) using leaf extracts of Populus ciliata as a reducing and stabilising agent. The synthesised NiO-NPs were characterised by ultraviolet-visible spectroscopy, Fourier transform infrared spectroscopy, powder X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. It was found that the synthesised NiO-NPs shapes varied, were highly crystalline, and had a face-centred cubic geometry. The calculated crystallite size of the synthesised nanoparticles was 44 nm. Moreover, the antibacterial activity of the synthesised NiO-NPs was also conducted against Gram-positive bacteria (Bacillus subtilis, Bacillus licheniformis) and Gram-negative bacteria (Escherichia coli and Klebsiella pneumoniae). Bacillus subtillus showed a maximum inhibition zone of 28.1±1.6 mm, whereas Klebsiella pneumonia showed a minimum inhibition zone of 9.2±0.5 mm. It was also found that the antibacterial activity increased with an increase in the concentration of NiO-NPs.

Abstract Introduction Posttonsillectomy pain results in significant morbidity to the patients. There is a disagreement in the literature regarding the use of local anesthetics during tonsillectomy. The aim of this placebo-controlled, double-blind study is to evaluate the effect of peritonsillar administration of local anesthetics. Objective To evaluate the role of intraoperative use of analgesics in tonsillar fossa and postoperative evaluation with visual analogue scale (VAS) scores in achieving pain relief after tonsillectomy procedure Methods In this study, 180 patients were randomized to 1 of the 6 groups: bupivacaine infiltration, lidocaine infiltration, normal saline infiltration, bupivacaine packing, lidocaine packing, and normal saline packing. Pain caused by speaking, swallowing, and on rest was assessed using VAS at 4, 8, 12, 16 hours, and at discharge. Results Significant analgesia was obtained in patients who received bupivacaine infiltration and packing compared with placebo (p < 0.05). The majority of the study subjects had no postoperative complications, and patients receiving bupivacaine infiltration required less additional analgesics in the first 24 hours after surgery. Conclusion We advocate the use of bupivacaine infiltration or packing immediately following the procedure to achieve adequate postoperative analgesia.

Abstract The research article is based on biodiesel synthesis by the transesterification of waste cooking oil with methanol in the presence of heterogeneous catalysts prepared from different marble. Eight samples of marble were successfully converted into potential catalysts by calcination. The thermal treatment of waste marbles at 300oC-1000oC converted the metal carbonates (CaCO3) to metal oxides (CaO). The calcined marble was analyzed by chemical tests, flame atomic absorption spectroscopy (FAAS), Fourier transform infrared spectroscopy (FT-IR), and X-ray diffraction studies (XRD). The presence of CaO in these catalysts made them highly reactive for biodiesel synthesis. The basicity and percentage of calcium in marble catalysts were calculated to know their basic strength. The transesterification was performed by fast stirring using waste cooking oil, methanol and nine different types of marble catalysts for 5 min at five different conditions, i.e., room temperature, hot plate stirring, solar ordinary irradiations, solar concentrated reflected irradiations and solar concentrated refracted irradiations. The solid catalysts were easily separated from the product for re-use. All marble catalysts were found to be active and basic except one namely silver pun (I). The production of biodiesel was confirmed by ASTM standards, TLC examination and by gas chromatography (GC).

A novel and sensitive chemiluminescence (CL) method was developed and validated for the determination of Citalopram in bulk dosage form and in pharmaceutical preparations. The method is based on the use of Cu²+-grafted oxidized multiwall carbon nanotubes (Cu/ox-MWCNTs). The weak CL signal arising from the reaction of an alkaline luminol-H2O2 system was significantly enhanced by the addition of citalopram in the presence of ox-MWCNTs/Cu²+. Furthermore, ox-MWCNTs/Cu²+ exhibited exceptional catalytic activity towards the oxidation of luminol in the luminol-H2O2 CL reaction. Multiwalled carbon nanotubes (MWCNTs) were characterized by scanning electron microscopy (SEM), which also showed the attachment of Cu²+ to MWCNTs. Various factors affecting CL intensity were carefully investigated and optimized for citalopram quantitation. The CL intensity was proportional to citalopram concentration in the range 0.2-8.0 mL-1, with a correlation coefficient of 0.996. The limit of detection (LOD) and limit of quantification were 2.29 X 10-5 mL-1 and 7.64 X 10-5 mL-1, respectively, and its reproducibility was satisfactory with a relative standard deviation (RSD) of 2.59 % (n = 5). The interference effects of common excipients were studied, and the developed method was effectively applied for the determination of citalopram in pure form and in pharmaceutical preparations. Percentage recoveries were calculated and ranged from 98.67 to 101.46 % for the pure form and from 97.38 to 101.72 % for pharmaceutical preparations.

ABSTRACT A simple and isocratic HPLC method with stability indicating nature was developed and then subsequently validated for simultaneous determination of ciprofloxacin and dexamethasone in pharmaceutical formulations, human serum and urine. Best chromatographic separations were attained within run time of 10 minutes using C8 as stationary phase and mixture of phosphate buffer and methanol (41:59 v/v) as mobile phase. The mobile phase was flowed at 1.5 mL min−1 with detection of both the analytes at 270 nm using photodiode array detector. Validation of the method was accomplished using specificity, linearity, accuracy, precision, robustness, LOD and LOQ. The method was found linear from 3-21 mg mL−1 for ciprofloxacin (r2 ≥ 0.999) and 1-7 mg mL−1 for dexamethasone (r2 ≥ 0.999). The %age recoveries of ciprofloxacin in spiked human urine and serum were ≥99% and ≥85% respectively, while for dexamethasone they were ≥97% in both matrices. The method proficiently separated the peaks of ciprofloxacin and dexamethasone from all types of interfering substances including degradation products/impurities with purity index ≥ 0.9998. The method thus was stability-indicating and can be employed for simultaneous analysis of ciprofloxacin and dexamethasone in complex matrices involving multiple components in the mixture.

Abstract In this study, conditions were optimized for development of a simple RP-HPLC method for simultaneous analysis of gatifloxacin and dexamethasone in different matrices like pharmaceuticals, human serum and urine. Good separation of gatifloxacin and dexamethasone from the induced degradation products was accomplished using C8 as stationary phase; 0.02 M phosphate buffer (pH 3.0) and methanol (42:58 v/v) as mobile phase. The concentration was measured with DAD at 270 nm. Linearity was observed in the range of 0.000040-0.000280 mol/L for gatifloxacin (r2≥0.999) and 0.000013-0.000091 mol/L for dexamethasone (r2≥0.999). Both the analyte peaks were completely separated from the peaks of induced degradation products as indicated by the peak purity index (≥0.9999 for both analytes). The optimized method is recommended to be used for concurrent analysis of gatifloxacin and dexamethasone in different matrices.

A stability-indicating RP-HPLC method is presented for determination of gatifloxacin and flurbiprofen in binary combination. Gatifloxacin, flurbiprofen and their degradation products were detected at 254 nm using a BDS Hypersil C8 (250 X 4.6 mm, 5 µm) column and mixture of 20 mM phosphate buffer (pH 3.0) and methanol 30:70 v/v as mobile phase. Response was linear over the range of 15-105 mg mL-1 for gatifloxacin (r² > 0.998) and of 1.5-10.5 mg mL-1 for flurbiprofen (r² > 0.999). The developed method efficiently separated the analytical peaks from degradation products (peak purity index > 0.9999). The method developed can be applied successfully for determination of gatifloxacin and flurbiprofen in human serum, urine, pharmaceutical formulations, and their stability studies.

Abstract A reversed phase high performance liquid chromatographic method has been developed for the simultaneous determination of cefaclor and ceftriaxone cephalosporin antibiotic. The developed method has been validated and applied to mixtures of the commercial formulation and spiked human plasma. A mediterranea C18 column (4.6 x 250 mm) was used with isocratic solvent delivery system and UV-visible detector. Different experimental parameters like solvent composition (acetonitrile: methanol: triethyl amine buffer 1:1:2 (v/v), flow rate of mobile phase (0.6 mLmin-1), pH of the buffer (7), and wavelength (260 nm) were optimized for effective separation and resolution of the analyte peaks. The separation was achieved in 6 min with retention times of 4.94 ± 0.056 min and 3.39 ± 0.022 min for cefaclor and ceftriaxone respectively. The linear range for both the studied drugs was found to be 0.5-250 μgmL-1 with r² of 0.9987 (cefaclor) and 0.9997 (ceftriaxone). The limit of detection (3.3 σ/S) was found to be 2.34 × 10-2 μgmL-1 and 1.70 × 10-2 μgmL-1, respectively, for cefaclor and ceftriaxone. Similarly limit of quantification (10σ/S) was 7.10 × 10-2 μgmL-1 for cefaclor and 5.15 × 10-2 μgmL-1 for ceftriaxone. The chromatographic procedure was applied to commercial formulations and spiked human plasma and the results were compared with literature HPLC method.

Resumen Se desarrolló un procedimiento para la determinación de cefaclor y ceftriaxona, dos antibióticos de la familia de cefalosporinas, por cromatografía de líquidos de alta resolución en fase inversa. El método fue utilizado en la determinación de dos compuestos en mezclas de formulaciones comerciales y en plasma sanguínea enriquecida con ambos. La separación se obtuvo en la columna Mediterranea C18 (4.6 x 250 mm) con elución isocrática. Los parámetros de separación cromatográfica y las condiciones de detección se establecieron con base en los experimentos tomando como criterio la resolución cromatográfica: la composición de fase móvil (acetonitrilo: metanol: tampón de trietilamnia 1:1:2 (v/v), flujo en la columna (0.6 mLmin-1), pH del tampón (pH 7) y la longitud de onda de detección (260 nm). En las condiciones propuestas, la separación de dos compuestos se obtuvo en 6 min con tiempos de retención 4.94±0.056 min y 3.39±0.022 min para cefaclor y para ceftriaxona, respectivamente. El rango lineal para ambos fármacos correspondió al intervalo 0.5-250 μgmL-1 con r² of 0.9987 (cefaclor) y 0.9997 (ceftriaxona). Los límites de detección (3.3 σ/S) fueron 2.34 × 10-2 μggmL-1 y 1.70 × 10-2 μgmL-1, respectivamente para cefaclor and ceftriaxona. Por su parte, los límites de quantificación (10 σ/S) fueron 7.10 × 10-2 μgmL-1 y 5.15 × 10-2 μgmL-1. El procedimiento desarrollado fue utilizado en la determinación de dos compuestos en formulaciones comerciales y en plasma sanguínea enriquecida, comparando los resultados con los reportados en bibliografía.

O presente estudo descreve o desenvolvimento e a subsequente validação de indicador de estabilidade simples e acurada por RP-HPLC para a determinação de esparfloxacino e dexametasona em formulações farmacêuticas na presença de produtos de degradação induzidos por estresse. Tanto os fármacos quanto os produtos de degradação induzidos pelo estresse foram separados em 10 minutos, utilizando coluna C8 e mistura de methanol e tampão fosfato 0,02 M, pH 3,0 (60:40 v/v, respectivamente) como fase móvel e detector de arranjo de diodo a 270 nm, A análise de regressão mostrou linearidade na faixa de 15-105 µg/mL para esparfloxacino e 5-35 µg/mL para a dexametsona. Todos os analitos foram resolvidos adequadamente com tailing aceitável. O pico de pureza dos dois foi maior que 0.9999, não mostrando picos de co-eluição. O método desenvolvido foi aplicado para a determinação simultânea de esparfloxacino e dexametasona em formulações farmacêuticas e para estudos de estabilidade.

The present study describes the development and subsequent validation of simple and accurate stability indicating RP-HPLC method for the determination of sparfloxacin and dexamethasone in pharmaceutical formulations in the presence of their stress-induced degradation products. Both the drugs and their stress-induced degradation products were separated within 10 minutes using C8 column and mixture of methanol and 0.02 M phosphate buffer pH 3.0 (60:40 v/v, respectively) as mobile phase at 270 nm using diode array detector. Regression analysis showed linearity in the range of 15-105 µg/mL for sparfloxacin and 5-35 µg/mL for dexamethasone. All the analytes were adequately resolved with acceptable tailing. Peak purity of the two drugs was also greater than 0.9999, showing no co-elution peaks. The developed method was applied for simultaneous determination of sparfloxacin and dexamethasone in pharmaceutical formulations for stability studies.

A simple, RP-HPLC method was established for determining moxifloxacin and ketorolac in pharmaceutical formulations. Moxifloxacin, ketorolac and their degradation products were separated using C8 column with methanol and phosphate buffer pH 3.0 (55:45 v/v) as the mobile phase. Detection was performed at 243 nm using a diode array detector. The method was validated using ICH guidelines and was linear in the range 20-140 µg mL-1 for both analytes. Good separation of both the analytes and their degradation products was achieved using this method. The developed method can be applied successfully for the determination of moxifloxacin and ketorolac.

The present study reports the development and validation of a simple, economic and sensitive HPLC method for the concurrent determination of naproxen and esomeprazole in pharmaceutical formulations. Isocratic chromatography was performed with C-18 column and mixture of phosphate buffer (pH 6.1) and acetonitrile in ratio of (40:60, v/v) at 1.5 mlmin-1. The eluents were monitored at 302 nm using UV detector. The method was isocratic in the range of 9.38 to 300 µgml-1 for naproxen and 0.5 to 16 µgml-1 for esomeprazole. Validation of the method was performed by testing parameters like linearity, accuracy, precision, robustness, specificity, LOD and LOQ values. In the specificity the drugs were subjected to forced degradation studies like acidic, basic, oxidative and thermal stresses. Both the analytes were separated within three minutes. As the method separates the degradation products produced during forced degradation studies from the active analytes so it can be used not only for regular determination of naproxen and esomeprazole but also for their stability studies.

A simple, sensitive and isocratic reverse phase high performance liquid chromatographic (RP-HPLC) method has been developed for the simultaneous determination of olmesartan medoxomil and amlodipine in pharmaceutical tablet formulations. HPLC analysis was carried out using reverse phase isocratic elution with aC18 column and amobilephase of 0.05 Mammonium acetate pH 6.8 and acetonitrile intheratio of 40:60, v/v. Detection of the analytes was achieved using UV detector at 239 nm. The retention times of olmesartan medoxomil and amlodipine were 2.50 and 3.94 respectively Linearity of the method was found to be in the concentration range of 16-112 µgml-1 for olmesartan medoximil and 4-28 µgml-1 for amlodipine. The correlation coefficient value was greaterthan 0.9999 for both the analytes. The method is suitable for the estimation of both the components simultaneously in pharmaceutical tablet formulations.