Development and Validation of UFLC-MS/MS Analytical Method for the Simultaneous Quantification of Antibiotic Residues in Surface Water, Groundwater, and Pharmaceutical Waste Water Samples from South India.

Antibiotic residues in pharmaceutical wastewater pose a significant environmental concern due to their potential role in fostering antimicrobial resistance. South Indian pharmaceutical companies produce a wide range of antibiotics. As a result, the industries that discharge water may include antibiotic residues, which could be harmful to the environment. In this study, a novel, quick, accurate, and sensitive approach for the simultaneous detection of 11 antibiotics was established, and triple quadrupole mass spectrometry, ultra-fast liquid chromatography-tandem mass spectrometry (UFLC-MS/MS), and selective solid-phase extraction (SPE) were used for validation. Utilizing a mixed mode reversed-phase/cation-exchange cartridge (SPE using Strata X, 33 µm), the single-cartridge extraction procedure was performed and validated. Relative standard deviations for most of the antibiotics ranged from 3.5 to 0.56 with recoveries ranging from 57 to 85%. The samples were injected into the UFLC-MS/MS apparatus at a volume of 10 µL for analysis. The auto sampler cooler temperature was kept at 150 °C, while the column temperature was kept at 40 °C. After validation, the technique was determined to be linear in the range of 2.0-1000.0 ng/mL. The retention period for antibiotics was between 1.2 and 1.5 min. Antibiotics transitions for multiple reaction monitoring| were between 235.1/105.9 and 711.5/467.9 m/z. The method of analysis took 2.5 min to run completely. Antibiotic residues were efficiently analyzed using the established analytical approach in pharmaceutical wastewater (influent and effluent), surface, and groundwater. Eleven antibiotics were found in the water samples during examination with concentrations ranging between 2.313 and 95.744 ng/L. The procedure was shown to be much more environmentally friendly than other contemporary methods based on the green analytical procedure index's evaluation of greenness. Blue applicability grade index tool indicated the developed method's practicality in comparison with that of other reported method.

Analytical Quality by Design-Assisted HPLC Method for Quantification of Canagliflozin and Stability Studies.

The present study is intended to develop the high-performance liquid chromatography (HPLC) method for the analysis of Canagliflozin using the analytical quality by design (AQbD) approach. The key parameters were methodically optimized with the help of factorial experimental design, and contours were plotted when investigated using Design Expert software. A stability-indicating HPLC technique was developed and validated for the quantitative estimation of Canagliflozin, and its stability was assessed using various forced degradation conditions. Successful separation of Canagliflozin was accomplished using a Waters HPLC system with a photo diode array (PDA) detector and Supelcosil C18 column (250 × 4.6 mm, 5 µm) and 0.2% v/v solution of trifluoroacetic acid in water/acetonitrile (80:20% v/v) as the mobile phase maintaining the flow rate at 1.0 mL/min. The detection wavelength was 290 nm, and Canagliflozin got eluted at 6.9 min with a run time of 15 min. Canagliflozin peak purity values in all degradation conditions indicated that the peak is homogeneous, and therefore this method can be considered stability-indicating. The proposed technique was found to be specific, precise (% RSD about 0.66%), linear (12.6-37.9 µg/mL), rugged (overall % RSD about 0.50%), and robust. The standard and sample solutions were stable after 48 h (cumulative % RSD about 0.61%). The developed AQbD-based HPLC method can be used for the assay of Canagliflozin in Canagliflozin tablets of regular production batches and stability samples.

Formulation of a thermo-sensitive hydro-gel for ulcerative colitis treatment.

Ulcerative colitis (UC) is a type of inflammatory bowel disease (IBD) that causes chronic intestinal inflammation in gastrointestinal (GI) tract, mainly in innermost lining of colonic mucosa. In any of the UC drug therapy regimens, maintaining remission is challenging and about 20-40% of patients don't respond to conventional UC medications, namely, amino salicylates, steroids and immunosuppressive drugs. These agents can weaken the patient's immune system thus enhancing the risk of infectious diseases. Therefore, in our exploration we probed to test marine-derived anti-inflammatory compounds as potential agents to treat UC. Fucoidan, a complex fucose-rich sulphated polysaccharide originated in edible brown algae with known anti-inflammatory properties was isolated from Turbinaria ornate. Collagen (Achillis tendon) is another agent that may provide a beneficial effect in wound healing and tissue regeneration. Collagen was also reported to possess anti-UC properties. Collagen has a limitation of being in solution form even at high concentrations. We therefore formulated fucoidan with collagen that underwent a sol-gel transition and yielded a gel like consistency in situ. This formulation showed sustained release of fucoidan for about 12 hours. The fucoidan, collagen and the fucoidan-collagen formulation were tested in the dextran sodium sulfate (DSS) induced colitis model in mice. In comparison to the vehicle treated group, fucoidan-collagen hydrogel formulation led to significant reduction in the clinical scores and rectal bleeding, which was higher than the reference standard, mesalamine and those seen with fucoidan and collagen given alone.

QbD-Based Development and Validation of Novel Stability-Indicating Method for the Assay and Dissolution of Garenoxacin in Garenoxacin Tablets.

BACKGROUND: Garenoxacin mesylate is a novel des-fluoro(6) quinolone, approved and marketed for human use in Japan under the name Geninax. OBJECTIVE: In this current work, a simple and stability-indicating method for the assay and dissolution of garenoxacin in garenoxacin tablets 200 mg was performed. New method developed for the particle size measurement of Garenoxacin mesylate Active Pharmaceutical Ingredient using Malvern 2000. METHODS: A quality by design (QbD)-based stability-indicating assay method was developed using 0.1% (v/v) formic acid in water and methanol (70:30). Using a photodiode array detector the peak purity of the garenoxacin peak for all degradation samples was studied. The biopharmaceutical classification system (BCS) solubility of garenoxacin mesylate active pharmaceutical ingredient (API) was studied by a modified shake flask method. A dissolution test method was developed using 0.1 N hydrochloric acid as the medium, United State Pharmacopoeia apparatus-II (paddle), revolution per minute (rpm) 50, temperature 37 ± 0.5°C and time 30 min. Liquid paraffin was used as the dispersant in the particle size measurement of garenoxacin mesylate API using the Malvern Mastersizer-wet method. RESULTS: The QbD-based RP-HPLC method was stability-indicating, simple, precise, and accurate. The assay method was linear over 12.5 to 75 µg/mL at the detection wavelength of 280 nm. A UV-based method was developed and validated for the dissolution of garenoxacin 200 mg tablets and the method was found to be linear over 2.9 to 34.2 µg/mL at 280 nm. Based on data, the dissolution tolerance for garenoxacin 200 mg tablets was proposed as Q not less than 80% at time 30 min (% drug released with respect to label claim (Q). The effect of garenoxacin mesylate API particle size in the tablet dosage form was studied using particles of 92 µm and 220 µm [90% of the total particles are smaller than this size (D90)] and it was found that there was no impact on the in vitro dissolution profile. CONCLUSION: The reported stability-indicating assay and dissolution test methods can be used in regular QC testing of garenoxacin 200 mg tablets. The Malvern particle size wet dispersion measurement method developed and validated for garenoxacin mesylate API is simple and robust. HIGHLIGHTS: A QbD based RP-HPLC method (using Design Expert Software version 11) was developed and studied peak purity of Garenoxacin peak using Photo Diode Array detector (for all degradation samples, control sample and standard solution) and the same method is validated following USP and ICH guidelines. LC-MS compatible volatile buffer solution is used in the preparation of the mobile phase for the novel stability-indicating RP-HPLC assay method.

Noncommunicable disease in rural India: Are we seriously underestimating the risk? The Nallampatti noncommunicable disease study.

AIM: To assess the prevalence of noncommunicable diseases in a true rural farming population in South India and compare the data with the landmark contemporary Indian Council of Medical Research-India Diabetes (ICMR-INDIAB) study. METHODS: Local Ethics Committee approval and informed consent was obtained from all participants. Inclusion criteria were participants, aged ≥20 and ≤85 years, from Nallampatti, a classical farming village from Tamil Nadu state, India. All participants were administered a detailed questionnaire, had anthropometric measurements including height, weight, and waist circumference. Bloods were drawn for random blood glucose, glycated hemoglobin (HbA1c), nonfasting lipid profile, Cystatin C, uric acid, and hemoglobin. All participants had carotid intima-media thickness (CIMT) done by high-resolution B-mode carotid ultrasound. RESULTS: More than 50% of the population had either diabetes or prediabetes based on HbA1c. Nearly, 40% of the population had hypertension with suboptimal control in those with known hypertension. Nearly, a third of the population had dyslipidemia, elevated cystatin C levels, and abnormal CIMT. The burden was higher than the comparable ICMR-INDIAB study in rural Tamil Nadu. CONCLUSION: One-third to one-half of this rural farming population is at risk of cardiovascular disease, with poor control of preexisting cardiovascular risk factors. Current Indian data may underestimate the risk in different ethnic populations and regions of India. Long-term follow-up of this cohort for the incident cardiovascular disease will shed light on the true cardiovascular risk in a typical South Indian rural farming population.