Predicting clinical entry point for thoracic epidural catheter insertion during paramedian approach: A prospective observational study.

Background and Aims: Thoracic epidural insertion has high failure rates in the mid-thoracic region due to steep angulation of oblique bending of spinous processes. The preferred skin puncture point for epidural needle insertion in the paramedian sagittal plane with respect to the superior/inferior tip of spinous process or inter-spinous cleft in the mid-thoracic region (T5-8) is not standard. The primary objective of this prospective observational study was to find the skin puncture point which had the best success rate for a successful epidural catheterization. Secondary objectives were to study the number of attempts and passes required to locate epidural space, incidence of failed epidural, and its relationship with patient characteristics and demographics. Material and Methods: After informed consent, 155 patients planned for general anesthesia with epidural analgesia in the mid-thoracic region were included in the trial. Patient demographics, the details of epidural attempts with respect to anatomical landmarks, distance from the midline, and number of passes in each attempt were noted. Epidural catheterization was considered successful after demonstrating dermatomal band of sensory blockade. Results: The success rate at different skin puncture sites was not statistically significant (P = 0.58). We found a failure rate of 12.9%. Failed epidural catheterization was significantly high in the age group >56 years (n = 62 and P = 0.007). Conclusion: In our study, none of the skin puncture points had a significant association with successful epidural insertion in mid-thoracic segments using a para-median approach.

A single-arm prospective interventional study to assess the efficacy of continuous bronchial cuff pressure monitoring to detect the displacement of lung isolation devices in elective thoracic surgeries.

Background and Aims: During proximal or distal migration of lung isolation device (LID), the bronchial cuff would move into a wider or narrower portion of the bronchus, leading to a decrease or increase in the cuff pressure, respectively. To test this hypothesis, we conducted a study to find out the efficacy of continuous bronchial cuff pressure (BCP) monitoring for detecting the displacement of LID. Methods: A single-arm interventional study was conducted including hundred adult patients undergoing elective thoracic surgeries using a left-sided LID. BCP was monitored in a continuous manner using a pressure transducer connected to the bronchial cuff of the LID. The position of the LID was assessed using a paediatric bronchoscope. Changes in the BCP were noted when the LID was moved intentionally in the left main bronchus (part 1) and during the surgery (part 2). Bronchoscopic confirmation was performed at the end of the surgery to note any uncaptured movement of the LID (part 3). Results: During part 1 of the study, BCP consistently decreased on the proximal movement and increased on the distal movement of the LID, although the magnitude of change was not constant. During part 2 of the study, sensitivity, specificity, positive predictive value, negative predictive value and accuracy of continuous BCP monitoring to detect the dislodgement of LIDs (n = 41) during the surgery were 97.6%, 40%, 76.9%, 88.9% and 78.7%, respectively. Conclusion: Continuous BCP monitoring is a useful and sensitive method for monitoring the position of left-sided LIDs in limited-resource settings.

Fine-tuning of MXene-nickel oxide-reduced graphene oxide nanocomposite bioelectrode: Sensor for the detection of influenza virus and viral protein.

Influenza viruses can cause epidemics through inter-human transmission, and the social consequences of viral transmission are incalculable. Current diagnostics for virus detection commonly relies on antibodies or nucleic acid as recognition reagent. However, a more advanced and general method for the facile development of new biosensors is increasing in demand. In this study, we report the fabrication of an ultra-sensitive peptide-based nanobiosensor using a nickel oxide (NiO)-reduced graphene oxide (rGO)/MXene nanocomposite to detect active influenza viruses (H1N1 and H5N2) and viral proteins. The sensing mechanism is based on the signal inhibition, the specific interaction between H1N1 (QMGFMTSPKHSV) and H5N1 (GHPHYNNPSLQL) binding peptides anchored on the NiO-rGO/MXene/glassy carbon electrode (GCE) surface and the viral surface protein hemagglutinin (HA) is the critical factor for the decrease in the peak current of the sensor. In this strategy, the NiO-rGO/MXene nanocomposite results in synergistic signal effects, including electrical conductivity, porosity, electroactive surface area, and active site availability when viruses are deposited on the electrode. Based on these observations, the results showed that the developed nanobiosensor was capable of highly sensitive and specific detection of their corresponding influenza viruses and viral proteins with a very low detection limit (3.63 nM of H1N1 and 2.39 nM for H5N1, respectively) and good recovery. The findings demonstrate that the proposed NiO-rGO/MXene-based peptide biosensor can provide insights for developing a wide range of clinical screening tools for detecting affected patients.

Strategies, advances, and challenges associated with the use of graphene-based nanocomposites for electrochemical biosensors.

Graphene is an intriguing two-dimensional honeycomb-like carbon material with a unique basal plane structure, charge carrier mobility, thermal conductivity, wide electrochemical spectrum, and unusual physicochemical properties. Therefore, it has attracted considerable scientific interest in the field of nanoscience and bionanotechnology. The high specific surface area of graphene allows it to support high biomolecule loading for good detection sensitivity. As such, graphene, graphene oxide (GO), and reduced GO are excellent materials for the fabrication of new nanocomposites and electrochemical sensors. Graphene has been widely used as a chemical building block and/or scaffold with various materials to create highly sensitive and selective electrochemical sensing microdevices. Over the past decade, significant advancements have been made by utilizing graphene and graphene-based nanocomposites to design electrochemical sensors with enhanced analytical performance. This review focus on the synthetic strategies, as well as the structure-to-function studies of graphene, electrochemistry, novel multi nanocomposites combining graphene, limit of detection, stability, sensitivity, assay time. Finally, the review describes the challenges, strategies and outlook on the future development of graphene sensors technology that would be usable for the internet of things are also highlighted.

Highly sensitive detection of anti-cancer drug based on bimetallic reduced graphene oxide nanocomposite.

Herein, we describe a high-performance electrochemical sensor for the detection of regorafenib (REG) using bimetallic Pd-Ru nanoparticles anchored on pomegranate peel extract (PPE) derived reduced graphene oxide (Pd-Ru/rGO). PPE was employed to neutralize the extremely acidic graphene then cast-off along with the metal precursor for the duration of the chemical reduction to accomplish well dispersed Pd-Ru nanoparticles. Bimetallic Pd-Ru/rGO nanocomposites were synthesized using a facile chemical reduction method. Under optimal conditions, based on the differential pulse voltammetric studies it has been confirmed that the fabricated sensors has good electrocatalytic activity toward the detection of REG, spanning over the linear dynamic range of 0.5-300 nM. Moreover, the sensor exhibited a low limit of detection of 1.6 nM and a limit of quantification of 4.8 nM. The electrochemical sensor unveiled admirable selectivity and sensitivity, reproducibility, and repeatability. The fabricated sensor was suitable for real sample analysis (pharmaceutical tablet, human blood plasm, wastewater) with satisfactory recovery. The strategy presented herein can be employed in the development of electrochemical sensors for other target analytes.

Assessing the Pain Reaction of Children and Evaluation of Efficacy of Buccal Infiltration with Articaine and Inferior Alveolar Nerve Block with Lignocaine for Pulp Therapy in Primary Mandibular Second Molars.

INTRODUCTION: Pain-free operating is of obvious benefit to the patient, it also helps the operator as treatment can be performed in a calm, unhurried fashion. Articaine hydrochloride has steadily grown in popularity, and studies have shown that articaine hydrochloride performs better than lidocaine due to an enhanced anesthetic efficacy. AIM AND OBJECTIVE: To assess the efficacy of buccal infiltration with articaine in achieving anesthesia for pulp therapy in primary mandibular second molars as compared with inferior alveolar nerve block (IANB) with lignocaine. MATERIALS AND METHODS: Thirty patients (4-8 years) with an indication of pulp therapy in at least two primary mandibular second molars were selected. Patients were randomly assigned to receive nerve block with lignocaine on the first appointment and buccal infiltration with articaine on the second appointment spaced 1 week apart. A single researcher injected local anesthetic for all the patients. Two researchers standing at a distance of 1.5 m recorded the pain scores and sound, eye, motor (SEM) scores. After the completion of the procedure, the patient was asked to record facial image (FI) score and Heft-Parker visual analog score (HP-VAS). RESULTS: The pain-related behavior scores were higher for IANB when compared with infiltration. Facial image and HP-VAS scores were higher for the lignocaine IANB group when compared with the articaine infiltration. CONCLUSION: With the increasing use of new delivery systems such as single tooth analgesia, a buccal infiltration with articaine provides an effective alternative, with minimal discomfort which would allow clinicians to avoid the use of IANB in children. HOW TO CITE THIS ARTICLE: Daneswari V, Venugopal Reddy N, Madhavi G, et al. Assessing the Pain Reaction of Children and Evaluation of Efficacy of Buccal Infiltration with Articaine and Inferior Alveolar Nerve Block with Lignocaine for Pulp Therapy in Primary Mandibular Second Molars. Int J Clin Pediatr Dent 2021;14(3):335-339.

Frailty and Nutritional Status among Urban Older Adults in South India.

The purpose of this study was to assess the prevalence of frailty and nutritional status among older adults. This population-based cross-sectional study was conducted in 163 subjects aged 60-88 years, from Hyderabad City, South India. Data were obtained on sociodemographic details and anthropometry and biochemical parameters. Dietary intake was assessed by a three-day 24 h dietary recall, and the probability of adequacy (PA) was calculated using the estimated average requirements. Frailty indicators were as follows: handgrip strength was measured by using a Jamar dynamometer, gait speed was measured by a ten-meter length walk test, and low physical activity level, weight loss, and exhaustion were assessed using a questionnaire. Among the study population, 20% of the participants were frail and 80% were nonfrail. The prevalence of frailty is higher in older (30.1%) than the younger (12.2%) age groups, and it is more so in women (32.4%) than in men (10.1%). The lower educational status and income were associated with frailty. The PA of most of the nutrients was low in the frail group. Noticeably, the mean PA (MPA) across the fourteen micronutrients was significantly higher in nonfrail (38%) compared to the frail group (25%). The prevalence of frailty was higher in the lowest tertile of most of the food groups and nutrient intake compared to the highest tertile. The study revealed a 20% prevalence of frailty among urban older adults and provided evidence that inadequate intake of nutrients is independently associated with frailty.

A Pt-free graphenaceous composite as an electro-catalyst for efficient oxygen reduction reaction.

Use of Pt-based electro-catalysts for the oxygen reduction reaction (ORR) is a major hindrance in large-scale application of proton exchange membrane fuel cells (PEMFCs). Hence, new, cost-effective and high performance electro-catalysts are required for the commercial success of PEMFCs. In this work, a Pt-free magnesium oxide (MgO) decorated multi-layered reduced graphene oxide (MLGO) composite is tested as an electro-catalyst for the ORR. The ORR activity of MgO/MLGO in terms of diffusion-controlled current density is found to be superior (6.63 mA per cm2-geo) than that of in-house prepared Pt/rGO (5.96 mA per cm2-geo) and commercial Pt/C (5.02 mA per cm2-geo). The applicability of less expensive MgO/MLGO not only provides a new electro-catalyst but also provides a new direction in exploring metal oxide-based electro-catalysts for the ORR.

Prevalence of vitamin deficiencies in an apparently healthy urban adult population: Assessed by subclinical status and dietary intakes.

OBJECTIVES: Studies in children and pregnant women consistently showed pandemic proportions of micronutrient deficiencies in the Indian subcontinent. However, vitamin deficiencies in apparently healthy adults are seldom recognized, hence the aim of this exploratory study was to assess their subclinical vitamin status and dietary intakes. METHODS: In all, 270 apparently healthy urban adults 30 to 70 y of age, from Hyderabad city, India participated in this study. Blood levels of vitamins (A, B1, B2, B6, total and active B12, D, and folate) and homocysteine were assessed. Anthropometric parameters were measured; dietary intake was obtained by food frequency questionnaire, and probability of adequacy (PA) was calculated by the estimated average requirement. RESULTS: Among the study population, the overall prevalence of deficiency of vitamin B2 was strikingly high (50%) followed by the vitamins B6 (46%), active B12 (46%), total B12 (37%), folate (32%), D (29%), B1 (11%), and A (6%). Hyperhomocysteinemia (HHcys) was widely prevalent (52%) in the study participants. In case of dietary intakes, PA was lowest for vitamin B12 (4%) and folate (9%) followed by vitamins A (22%), B2 (33%), B6 (30%), and B1 (59%). The mean PA of these vitamins was noticeably low (28%). The unadjusted logistic regression analysis found men and those with a deficiency of folate and total and active B12 to be at higher risk for HHcys. In the adjusted model, the risk for active B12 deficiency almost doubled. CONCLUSION: The study demonstrated a high prevalence of multiple subclinical vitamin deficiencies, dietary inadequacies, and HHcys, which are possible risk factors for disease burden among apparently healthy adults.

Effect of surfactants and hydrophilic polymers on the stability of an antihypertensive drug candesartan cilexetil: Evaluation by HPLC.

OBJECTIVES: The objective of this study is to investigate the effect of surfactants (polysorbate 80 and sodium lauryl sulphate) and hydrophilic polymers (polyvinylpyrrolidone and polyethylene glycol 6000) on the stability of candesartan cilexetil under isothermal stress conditions (100°C, 48h). METHODS: HPLC method was employed to evaluate the drug content and formation of degradation products in stress samples. Drug and degradation products were separated on Hypersil BDS C18 (250×4.6mm, 5µ) column using acetonitrile-water (pH 2.8) in the ratio of 85:15% v/v as a mobile phase. RESULT: Similar degradation behaviour of drug was observed with polyvinylpyrrolidone, polyethylene glycol 6000 and polysorbate 80; four common degradation peaks were observed at the retention time of 3.7, 4.5, 7.8 and 11minutes. One extra common degradation peak of very low intensity was also observed with polyethylene glycol 6000 and polysorbate 80 at the retention time of 4.2min. The drug was eluting at the retention time of 5.4min. In the case of sodium lauryl sulphate, two prominent degradation peaks were observed at the retention time of 3.7 and 13.25min along with few very low-intensity degradation peaks. CONCLUSION: The drug showed 41%, 64%, 72% and 98% degradation in presence of polyvinylpyrrolidone, polyethylene glycol 6000, polysorbate 80 and sodium lauryl sulphate, respectively.

Anti-arthritic activity of a classical Ayurvedic formulation Vatari Guggulu in rats.

In India, Vatari Guggulu has been traditionally used in the Ayurvedic system of medicine to treat rheumatoid arthritis (RA). The current study was undertaken to evaluate anti-arthritic activity of alcoholic extract of Vatari Guggulu in rats. Arthritis was induced by administration of formaldehyde (2%v/v) or Complete Freund's Adjuvant (CFA) into the sub-plantar surface of left hind paw of the animals. The extract was administered to the rats by oral gavages in different doses. Joint swelling was measured in formaldehyde induced arthritis. Various physical, biochemical and histopathological parameters were determined in CFA induced arthritis. Vatari Guggulu extract (VGE) produced significant (P < 0.05) inhibition of joint swelling in both formaldehyde and CFA induced arthritis. The treatment also brought to normalcy the increased white blood cell (WBC) count, rheumatoid factor (RF), erythrocyte sedimentation rate (ESR), cholesterol, triglycerides and LDL with an enhancement of haemoglobin (Hb) levels and red blood cell (RBC) count. These effects were found to be dose dependent. These effects were comparable with standard drug indomethacin. Histo-pathological studies of the ankles of VGE treated animals exhibited significant improvements. VGE did not show any toxic symptoms even at a dose of 2000 mg/kg in acute toxicity studies on rats. Thus, Vatari Guggulu, a classical Ayurvedic formulation of the Indian System of Medicine, exhibited significant anti-arthritic activity in formaldehyde and CFA induced arthritis in rats. This study corroborates the claims of Ayurveda on Vatari Guggulu.

Green chemical approach towards the synthesis of SnO2 NPs in argument with photocatalytic degradation of diazo dye and its kinetic studies.

There are variety of effluents are dumped or directly discarded into atmosphere due to drastic industrialization which leads to damages in living organisms. To prevent many type of environmental defects our research group focused to synthesis material which degrades toxic substance like dyes with the help of ecofriendly synthesis. We have synthesized Tin oxide nanoparticles (SnO2 NPs) using aqueous extract of Catunaregam spinosa (C. spinosa) root barks. Bio-inspired synthesized SnO2 NPs were monitored by analytical characterization which inferred that SnO2 NPs resulted in shape of spherical, with size average of 47±2nm. Further bio-green synthesized SnO2 NPs were subjected to degrade toxic Congo red dye, which results in higher percentage of degradation with the K value of 0.9212 which obeys pseudo-first order reaction kinetics. This report said to be novel due to null report on SnO2 NPs synthesized from C. spinosa root bark aqueous extract which also stated to be simplest, cheaper and non-toxic while compare to other methods. Further to identify the metabolites which is present in the aqueous extract were identified through Gas Chromatography and Mass Spectrometry with methanol as a solvent results that 7-hydroxy-6-methoxy-2H-1-benzopyran-2-one contains higher area percentage of 67.47 with the retention time (RT) of 18.660.

Effect of ethanol extract of an ayurvedic preparation (Pathyadya Churna) on arthritis in rats.

OBJECTIVES: To study the anti-arthritic activity of Pathyadya Churna ethanol extract (PCE) in rats. MATERIALS AND METHODS: Formaldehyde (2% v/v) or complete Freund's adjuvant (CFA 0.l mL) was injected in the left hind paw of male Wistar rats to develop arthritis. These rats were treated with three doses (135, 270, and 540 mg/kg) of PCE and one dose (10 mg/kg) of indomethacin. Anti-arthritic activity of the extract was assessed by noting paw volumes, rheumatoid factor (RF), blood parameters, and histological changes. RESULTS: PCE treatment reduced paw swelling in arthritis caused by both formaldehyde and CFA. In CFA-treated rats, a significant decrease (P < 0.001) was seen in hemoglobin (13.92 g/dL to 9.97 g/dL), red blood cell count (7.32 million/mm(3) to 6.58 million/mm(3)), and packed cell volume (44.04% to 30.56%). There were also significant (P < 0.001) elevations in white blood cell count (8220/-11,420/mm(3)), platelets (2.46-4.15 lakhs/mL), erythrocyte sedimentation rate (3.76-8.03/60 min), RF (7.17-26.77 IU/mL), triglycerides (71.69-96.60 mg/dL), total cholesterol (96.85-145.05 mg/dL), low-density lipoprotein (53.11-109.60 mg/dL), and very low-density lipoprotein (14.34-19.32 mg/dL). In CFA-induced arthritic rats, high-density lipoprotein decreased significantly (29.40 mg/dL to 16.13 mg/dL). Marked changes were noted in the histology of ankles. Treatment with PCE significantly reversed all these hematological and histological changes in a dose-dependent manner. CONCLUSIONS: PCE has a significant anti-arthritic activity in rats and is free from toxic effects.

Determination of dopamine in presence of ascorbic acid and uric acid using poly (Spands Reagent) modified carbon paste electrode.

In this paper, we have fabricated a modified carbon paste electrode (CPE) by electropolymerisation of spands reagent (SR) onto surface of CPE using cyclic voltammetry (CV). The developed electrode was abbreviated as poly(SR)/CPE and the surface morphology of the modified electrode was studied by using scanning electron microscopy (SEM). The developed electrode showed higher electrocatalytic properties towards the detection of dopamine (DA) in 0.1M phosphate buffer solution (PBS) at pH7.0. The effect of pH, scan rate, accumulation time and concentration of dopamine was studied at poly(SR)/CPE. The poly(SR)/CPE was successfully used as a sensor for the selective determination of DA in presence of ascorbic acid (AA) and uric acid (UA) without any interference. The poly(SR)/CPE showed a good detection limit of 0.7 µM over the linear dynamic range of 1.6 µM to 16 µM, which is extremely lower than the reported methods. The prepared poly(SR)/CPE exhibited good stability, high sensitivity, better reproducibility, low detection limit towards the determination of DA. The developed method was also applied for the determination of DA in real samples.

Development and validation of a systematic UPLC-MS/MS method for simultaneous determination of three phenol impurities in ritonavir.

A stability indicating gradient reverse phase UPLC-MS/MS method was developed and validated for the simultaneous determination of three phenol impurities in ritonavir drug substance. The chromatographic separation was performed on Acquity UPLC BEH C18 column (100 mm × 2.1 mm, 1.7 µm) using gradient elution of 0.05% ammonia in methanol and 5.0 mM ammonium acetate buffer (30:70, v/v) at a flow rate of 0.2 mL/min. Both negative and positive electrospray ionization (ESI) modes were operated simultaneously for the quantification of three phenol impurities. The total run time was 11 min, within which ritonavir and its three impurities were well separated. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection, limit of quantification, accuracy, precision and robustness. The calibration curves showed a good linearity over the concentration range of 0.3-1.5 ppm for phenol and 0.1-1.5 ppm for both 4-nitrophenol and N-phenoxycarbonyl-L-valine (NPV). The determination coefficient obtained was >0.9998 in each case. The method had very low limit of detection (LOD) and limit of quantification (LOQ) and the accuracy lies between 97.8% and 103.2% for all the three phenol impurities. The developed method was successfully applied for five formulation batches of ritonavir to determine its phenol impurities.

The modern integrated anaesthesia workstation.

Over the years, the conventional anaesthesia machine has evolved into an advanced carestation. The new machines use advanced electronics, software and technology to offer extensive capabilities for ventilation, monitoring, inhaled agent delivery, low-flow anaesthesia and closed-loop anaesthesia. They offer integrated monitoring and recording facilities and seamless integration with anaesthesia information systems. It is possible to deliver tidal volumes accurately and eliminate several hazards associated with the low pressure system and oxygen flush. Appropriate use can result in enhanced safety and ergonomy of anaesthetic delivery and monitoring. However, these workstations have brought in a new set of limitations and potential drawbacks. There are differences in technology and operational principles amongst the new workstations. Understand the principles of operation of these workstations and have a thorough knowledge of the operating manual of the individual machines.

A selective and sensitive UPLC-MS/MS approach for trace level quantification of four potential genotoxic impurities in zolmitriptan drug substance.

The pivotal task of pharmaceutical industry is to separate and quantify the potential genotoxic impurities (PGIs) rising from the process of drug production. For trace level quantification of these PGIs we need to develop sensitive and selective analytical methods. APP, NPA, NPP and MNA have been highlighted as PGIs in zolmitriptan. A sensitive and selective UPLC-MS/MS method has developed for identification and quantification of four PGIs viz. APP, NPA, NPP and MNA in zolmitriptan. The method utilizes Hypersil BDS C8 column (50 mm × 4.6 mm, 3.0 µm) with electrospray ionization in selected ion recording (SIR) mode for quantitation of four PGIs. The method was validated as per International Conference on Harmonization (ICH) guidelines and is able to quantitate APP at 0.1 ppm and NPA, NPP and MNA at 0.15 ppm with respect to 5.0mg/mL of zolmitriptan. The proposed method is specific, linear, accurate and precise. The method is linear in the range of 0.1-2.0 ppm for APP and 0.15-2.0 ppm for NPA, NPP and MNA, which matches the range of LOQ-200% of estimated permitted level (1.0 ppm). The correlation coefficient obtained was >0.999 in each case. The impurities were not present in the studied three pure and formulation batches of zolmitriptan. The accuracy of the method was ranged between 98.1 and 102.8% for four PGIs. This method is a good quality control tool for quantitation of four APP, NPA, NPP and MNA PGIs at very low levels in zolmitriptan.

Systematic Approach for Trace Level Quantification of 2-N-butyl-4-spirocyclopentane-2-imidazole-5-one Genotoxic Impurity in Irbesartan Using LC-MS/MS.

2-N-butyl-4-spirocyclopentane-2-imidazoline-5-one has been highlighted as a potential genotoxic impurity in irbesartan. A sensitive LC-MS/MS method was developed and validated for the determination of 2-N-butyl-4-spirocyclopentane-2-imidazoline-5-one in irbesartan. Good separation between 2-N-butyl-4-spirocyclopentane-2-imidazoline-5-one and irbesartan was achieved with Symmetry C18 (100×4.6 mm, 3.5 µm) column using 65:35 v/v mixture of 0.1% formic acid and acetonitrile as mobile phase with a flow rate of 0.7 ml/min. The proposed method was specific, linear, accurate, and precise. The calibration curve shows good linearity over the concentration range of 0.1-2.0 µg/ml, which matches the range of limit of quantitation-20×limit of quantitation of estimated permitted level (1.0 µg/ml) of 2-N-butyl-4-spirocyclopentane-2-imidazoline-5-one. The method was validated as per International Conference on Harmonization guidelines and was able to quantitate 2-N-butyl-4-spirocyclopentane-2-imidazoline-5-one impurity at 1.0 µg/ml with respect to 2 mg/ml of irbesartan. 2-N-butyl-4-spirocyclopentane-2-imidazoline-5-one was not present in the three studied pure and formulation batches of irbesartan and the developed method was a good quality control tool for quantitation of 2-N-butyl-4-spirocyclopentane-2-imidazole-5-one at very low levels in irbesartan.

Method development and validation study for quantitative determination of 2-chloromethyl-3,4-dimethoxy pyridine hydrochloride a genotoxic impurity in pantoprazole active pharmaceutical ingredient (API) by LC/MS/MS.

A sensitive and selective liquid chromatographic-tandem mass spectrometric (LC/MS/MS) method was developed and validated for the trace analysis (>1 ppm level) of 2-chloromethyl-3,4-dimethoxy pyridine hydrochloride a genotoxic impurity in pantoprazole sodium drug substances. LC/MS/MS analysis of 2-chloromethyl-3,4-dimethoxy pyridine hydrochloride was done on Hypersil BDS C18 (50 mm × 4.6 mm) 3 µm column and 10 mM ammonium acetate in 1000 mL of water was used as buffer. The mobile phase used was in the ratio of buffer-acetonitrile (79:21, v/v). The flow rate was 1.0 mL/min and elution was monitored at 210 nm. The method was validated as per International Conference on Harmonization (ICH) guidelines. LC/MS/MS is able to quantitate up to 0.3 ppm of 2-chloromethyl-3,4-dimethoxy pyridine hydrochloride.

Development and validation of a RP-HPLC method for the simultaneous determination of Embelin, Rottlerin and Ellagic acid in Vidangadi churna.

Vidangadi churna is a popular Ayurvedic formulation described in the chapter Krimicikitsa of the Ayurvedic literature Cakradatta for the treatment of Krimiroga. The preparation is a composite mixture of the fine powder of fruits of Vidang (Embelia ribs), glandular trichomes of the fruits of Kamala (Mallotus philippensis), mature fruits of Harde (Terminalia chebula), Saindhava and Yavakshara. The use of reversed phase C18 column eluted with gradient mobile phase of acetonitrile and water enabled the efficient separation of the chemical markers in 22 min. Validation of the method was performed in order to demonstrate its selectivity, accuracy, precision, repeatability and recovery. All calibration curves showed good linear correlation coefficients (r2>0.995) within the tested ranges. Three markers in Vidangadi churna were quantified with respect to Embelin (0.647%, w/w), Rottlerin (4.419%, w/w), and Ellagic acid (0.459%, w/w). Intra-and inter-day RSDs of retention times and peak areas were less than 3.12%. The recoveries were between 99.66% and 102.33%. In conclusion, a method has been developed for the simultaneous quantification of three markers in Vidangadi churna. The RP-HPLC method was simple, precise and accurate and can be used for the quality control of the raw materials as well as formulations.