Analytical lifecycle management oriented development and validation of a new stability-indicating ultra-fast liquid chromatographic method: case study of Glycopyrrolate

A new stability-indicating liquid chromatographic method was developed and validated for the estimation of glycopyrrolate in pharmaceutical formulations. A contemporary approach to analytical life-cycle management was followed to develop a robust and reliable chromatographic method. Scouted method variables such as % methanol, the strength of tetra butyl ammonium hydrogen sulfate and mobile phase flow rate were optimized using the design of experiment approach and their effect on critical quality attributes was studied. The critical quality attributes viz. retention time, theoretical plate count and symmetry factor were highly influenced by the three critical method variables. Optimum chromatography was attained on a C-18 column with a mobile phase methanol: 10 mM tetra butyl ammonium hydrogen sulfate (80:20, v/v) flowing at 1.0 mL.min-1. Chromatographic method specificity was ensured by degrading the drug forcefully. Validation studies postulated method acceptability and suitability for estimating glycopyrrolate in both bulk as well as injection formulation. Results for parameters viz. linearity (5-250 µg.mL-1), accuracy (>99%) and precision (<2%) advocated method reliability. Overall the method was reliable and of optimum quality and, possess the potential of application in routine and bio-analytical purposes

Fine-needle Aspiration Cytology in Diagnosing Soft-tissue Swellings: A Retrospective Study

Aim: To determine the accuracy of fine-needle aspiration cytology (FNAC) in diagnosing soft-tissue swellings. Materials and Methods: A retrospective study was conducted over a period of 2 year (September 2015 to September 2017), which included 96 patients who presented with soft-tissue swelling to the surgical outpatient department. All the above patients were subjected to FNAC and were operated for the swelling; their histopathological reports were correlated with the preoperative FNAC report to determine the accuracy of FNAC in correctly diagnosing the soft-tissue swelling. The data in this study were analyzed using statistical analysis system software. Results: Majority of the patients were in the 3rd decade of life and the number of females was more than males. The accuracy of FNAC in diagnosing soft-tissue swelling in the present study was found to be 77.78%. Conclusion: FNAC is a safe, quick, and inexpensive technique in diagnosing soft-tissue swelling with a high degree of accuracy.

Inguinal Swellings Mimicking Hernia in Females: A Retrospective Study.

Background: Inguinal hernia results from the failure of embryonic closure of the deep inguinal ring and is the most common cause of swelling in the groin region. However, an inguinal hernia is not the only cause for swelling in that region. Objectives: The main aim and objective of this study were to evaluate female patients with swellings in the inguinal region in terms of incidence, clinical presentation, age distribution, and differential diagnosis. Methods: The present clinical study was carried out at the Department of General Surgery; Shimoga Institute of Medical Sciences, Shimoga from March 2014 to March 2015. All the patients were thoroughly investigated, and surgical procedures were done. Results: Among the 10 cases studied, 6 cases were the regular inguinal hernia and the rest 4 cases were a subcutaneous lipoma. The ultrasonography of the part had revealed it has hernias. Surgical procedures were done and specimens obtained were sent to histopathological examination. Conclusion: The present study reveals that all inguinal swellings need not be a hernia and it can be due to other causes also and ultrasonography of the part is not the conclusive diagnostic tool.

Prospective clinical study of surgical management of varicose veins of lower limb and its complications.

Background: Varicose veins of the lower extremities are the most common peripheral vascular disease and their treatment is as old as mankind. This prospective clinical study of surgical management of varicose vein was conducted to study the age, sex and occupational distribution of varicose veins of lower limb. Evaluations of clinical features and surgical methods of treatments that were in practice in the management of varicose veins in terms of recurrence and symptoms improvement were also studied. Methods: Two years prospective study was conducted in our institution from May 2007 to April 2009. During this period 62 cases of varicose veins of lower limbs were admitted to our hospital of which 50 cases were selected and were studies in detail. After thorough clinical examination and relevant investigation they are all subjected to surgical management. Results: Out of 50 cases studied, 21 (42%) had only long saphenous vein involvement, 7 (14%) had short saphenous vein involvement and in 5 (10%) cases both short and long saphenous system were involved. In addition to long saphenous vein involvement, incompetent perforators were present in 17 (34%) cases. Among them prominent veins and pain were the main complain in 38 (78%) patients. Itching and pigmentation were present in 4 (8%) patients. Ankle edema was present in 6 (12%) patients. Pain and ulceration of lower leg were present in 2 (4%) patients. After clinical assessment appropriate surgical procedures were followed for each of patients. These cases were followed for 3 year durations. Out of 50 patients 7 (14%) patients had recurrence of varicose vein. 7 (14%) patient complained of recurrence of pain after 2 years of surgery but no appearance of varicose vein. One patient (2%) complained of persistence of pigmentation after surgery. 2 (4%) patients complained of persistence of ankle edema and there was complete healing of ulcer which was present earlier. Conclusions: Commonest age group of varicose vein of lower limb was 20 to 40 years. Definite relationship exists between the occupation and the incidence of varicose veins. The patients were in the occupation which required standing for long time had the higher chances of varicose vein. Severity of the symptoms is not proportional to the duration of varicose veins. The involvement of long saphenous vein is more common than the short saphenous vein. Since our study shows very low percentage of recurrence and symptoms related to varicose vein the surgical line of treatment is an ideal treatment for varicose vein. For incompetent perforators, sub-fascial ligation appears to be a better method of treatment than extra fascial ligation. Because in the former all the perforators could be visualized and dealt with, while in the latter there were chances of missing one or two perforators. If cases are selected properly with good operative technique the complications are negligible

Prospective study of comparison between the ultrasonography with the plain radiography in the diagnosis of pneumoperitoneum of hollow viscus perforation.

Background: This study was conducted to compare the plain radiography with the abdominal ultrasonography in the detection of pneumoperitoneum in suspected cases of hollow viscus perforation. Methods: A total number of 60 patients with suspected hollow viscus perforation were studied. All the patients had undergone plain radiography (Erect x-ray abdomen and left lateral decubitus views), ultrasonography and exploratory laparotomy. The investigational findings were compared with that of laparotomy findings. They were compared in terms of their sensitivity, specificity, predictive value of a positive and negative results and their percentage of false positive and false negative results. Results: Of the 60 patients, who underwent laparotomy, 57 had hollow viscus perforation. Out of 3 non-hollow viscus perforated cases 2 had appendicular perforation and 1 had mesenteric lymphadenitis. In the diagnosis, ultrasonography vs. radiography, their respective parameters were sensitivity (73.7% vs. 80.7%), specificity (66.7% each), predictive value of a positive test (97.7% vs. 97.9%), predictive value of a negative test (11.8% vs. 15.4%), percentage of false negative (26.3% vs. 19.3%) and percentage of false positive (33.3% each). Conclusion: In detection of pneumoperitoneum plain radiography appears to be more sensitive than ultrasonography with comparable specificity. Ultrasonographic finding of pneumoperitoneum is considered as an added finding.

A RP-HPLC Method Development and Validation for the Estimation of Gliclazide in bulk and Pharmaceutical Dosage Forms.

A simple, selective, linear, precise and accurate RP-HPLC method was developed and validated for rapid assay of Gliclazide in pharmaceutical dosage form. Isocratic elution at a flow rate of 1.2 ml min -1 was employed on a symmetry C18 column at ambient temperature. The mobile phase consisted of methanol: phosphate buffer 50:50 (V/V). The UV detection wavelength was at 210 nm. Linearity was observed in concentration range of 1-100 μg/mL. The retention time for Gliclazide was 3.25 min. The method was validated as per the ICH guidelines. The proposed method can be successfully applied for the estimation of Gliclazide in pharmaceutical dosage forms.

Synthesis and biological evaluation of new 4-bromo-3, 5-diaryl-1-phenyl-2-pyrazoline derivatives as antioxidant and anti-inflammatory agents.

A number of substituted 1, 3-diphenylprop-2-en-1-one were prepared by Claisen-Schmidt condensation of p-substituted acetophenone with o,m,psubstituted aryl aldehydes which undergoes bromination and subsequent cyclization with phenyl hydrazine to yield 4-bromo-3(substituted phenyl)-5(substituted phenyl)-1-phenyl-2-pyrazoline (3a-l). The structures of compounds were confirmed by elemental analysis, IR, 1HNMR and mass spectral data. The synthesized compounds (3a-l) were screened for anti-oxidant and anti-inflammatory activity. The free radical scavenging properties were screened by using ascorbic acid as standard antioxidant. Free radical scavenging activity was evaluated using 1,1-diphenyl-2-picryl hydrazyl (DPPH) free radical. The antioxidant activity of compound 3b was found to be the strongest. The IC50 values of the synthesized compounds ranged between 8.87 and 81.07 (μg mL-1). The anti-inflammatory activities were evaluated by using diclofenac sodium as a standard dug. All the compounds (20mg/kg po) possess significant anti-inflammatory activity, as reflected by their ability to provide protection (66-99%) against carragenan induced edema in rat paw. The anti-inflammatory activity of compound 3g was found to be the highest. The safety of substituted bromo-pyrazolines is reflected by toxicity studies.

Prevalence of Candida in the oral cavity of diabetic subjects.

OBJECTIVE: Estimation of prevalence of Candida in the oral cavity of diabetic and non-diabetic subjects. MATERIAL AND METHODS: One hundred and three subjects of diabetes mellitus (49 Type 1 diabetes mellitus and 54 Type 2 diabetes mellitus) and one hundred non-diabetic subjects (control) were studied. RESULTS: 41(83.67%) out of 49 Type 1 diabetes mellitus, 37(68.52%) out of 54 Type 2 diabetes mellitus and 27(27%) out of 100 in non-diabetic subjects were found to carry Candida in their oral cavity. Colony Forming Unit (CFU) of Candida in the oral cavity ranking in groups was Type 1 diabetes mellitus > Type 2 diabetes mellitus > non-diabetic subjects. CONCLUSION: Colonization and carriage of Candida in the oral cavity was found to be higher in diabetic subjects than in non-diabetic subjects. However anti-diabetic therapy and glycaemic control in diabetes were found to bear no relation with carriage of Candida in the oral cavity.