Mean Recovery Research Articles

An innovative phase I study in healthy subjects to determine the mass balance, elimination, metabolism, and absolute bioavailability of mitapivat.

Mitapivat, a first-in-class, oral, small-molecule, allosteric activator of the red blood cell-specific form of pyruvate kinase (PKR), was approved for the treatment of hemolytic anemia in adults with pyruvate kinase (PK) deficiency. In this phase I mass balance study in healthy males, we administered a single ~120 mg oral dose of [14 C]mitapivat and a concomitant intravenous ~0.1 mg microdose of [13 C6 ]mitapivat. We determined (1) the routes of total radioactivity excretion, including the mass balance of total radioactivity in urine and feces; (2) the pharmacokinetics of mitapivat and [13 C6 ]mitapivat in plasma and total radioactivity in whole blood and plasma; (3) the absolute oral bioavailability of mitapivat; and (4) the metabolite profiles in plasma and excreta. Mean recovery of the radioactive dose was 89.1% (49.6% in urine and 39.6% in feces). [14 C]Mitapivat was rapidly absorbed and extensively metabolized as <4% of the total radioactive dose was excreted unaltered in urine and feces. Mean absolute oral bioavailability was 72.7%. A total of 17 metabolites were identified. Mitapivat accounted for 57% and 34% of plasma radioactivity in AUC0-24 and AUC0-72 pooled samples, respectively. The remaining radioactivity was attributable to several metabolites, each representing <10% of the total radioactivity in pooled samples; none were disproportionate metabolites as defined by the US Food and Drug Administration and International Conference on Harmonisation M3 guidelines. Metabolite structures suggest that the primary metabolic pathways for [14 C]mitapivat in humans include N-dealkylation of the cyclopropylmethyl moiety, oxygenation of the quinoline-8-sulfonamide, oxidation/unsaturation, scission of the piperazine moiety, and amide hydrolysis.

A Validated RP-HPLC Method for Simultaneous Assay Determination and UV-Spectrophotometric Method for Dissolution Estimation in Film-Coated Tablets Containing Cefixime and Clavulanic Acid

A simple and novel reverse phase high performance liquid chromatography (RP-HPLC) method was developed for the simultaneous assay estimation of film coated tablets incorporating clavulanic acid (CVA) and cefixime (CFX). Furthermore, the same method was also applied in order to assess the dissolution of CVA while a UV spectroscopic method was produced to examine the drug release of CFX. In this research, an analytical column used was C18 (4.6-mm × 25-cm); 5-μm. Moreover, the mobile phase was prepared by completely dissolving 3.408 gm of disodium hydrogen phosphate in 800 mL of water (HPLC grade), 200 mL methanol was added in (20:80 v/v) it and then finally pH was adjusted to 6.0 using orthophosphoric acid. In addition, flow rate, detecting wavelength, and run time were 1.0 mL/min, 220 nm, and 15 minutes, respectively. Furthermore, the maximum absorption of CFX was obtained at 288 nm thereby this wavelength was optimized for the dissolution estimation of CFX by UV spectroscopy. The validation parameters were validated according to the specifications and guidelines of the international conference on harmonization (ICH) prior to evaluating both assay and dissolution of CVA and CFX. In case of assay estimation, the findings of the linearity revealed a linear interrelation of concentration between 0.16 - 0.25 mg/mL for both CVA and CFX. Similarly, the calibration curve was linear between the concentration range of 0.03 – 0.045 mg/mL and 0.004 – 0.006 mg/mL, respectively for dissolution determination. Additionally, the value of LOD and LOQ of CVA for assay evaluation was obtained 0.011 and 0.033 μg, respectively. The accuracy of the developed method was assessed by determining recovery studies and the mean recovery of CVA and CFX obtained 99.35% and 100.50%, respectively at 100% spiked level for assay analysis. The repeatability evaluation for assay and dissolution demonstrated that the optimized method is precise within the appropriate range and the RSD% was observed lower than 2.0%. In addition, results of different validation parameters including study of solution stability were achieved within the suitable limit as well.

Development and validation of analytical method for determination of valproate and valproic acid in bulk and pharmaceutical dosage form by using RP-HPLC

A New RP-HPLC Method for the Simultaneous Estimation of Valproate and Valproic acid in bulk and its Pure and Pharmaceutical Dosage Form as per ICH Guidelines. The Present work was to develop a simple, fast, accurate, precise, reproducible, Reverse Phase High Performance Liquid Chromatographic Method for simultaneous estimation of Valproate and Valproic acid in pure and combined dosage form. Chromatographic separation was done using Symmetry ODS C18 column having dimension of 4.6×250mm having particle size of 5.0µm, with mobile phase consisting of Acetonitrile: Methanol in the ratio 65:45v/v, flow rate was adjusted to 1ml/min and detection wavelength at 256nm. The retention times of Valproate and Valproic acid was found to be 2.256 and 5.427 mins. The proposed method has been validated for accuracy, precision, linearity; robustness and range were within the acceptance limit according to ICH guidelines. Linearity for Valproate and Valproic acid was found in range of 6µg-14µg and 18µg-42µg and correlation coefficient was found to be 0.999 and 0.999% RSD for intermediate precision was found to be 0.5 and 0.3, for repeatability was 0.4 and 0.1, % mean recovery for Valproate and Valproic acid was found to be 101.326% and 100.501% respectively. The method was found to be robust even by change in the mobile phase ±2% and in more and less flow conditions. The developed method can be successfully employed for the routine analysis of Valproate and Valproic acid in bulk and Pharmaceutical dosage forms.&#x0D;

Vortex-assisted dispersive liquid-liquid microextraction based on the hydrophobic deep eutectic solvent-based ferrofluid for extraction and detection of myclobutanil.

A vortex-assisted dispersive liquid-liquid microextraction (VA-DLLME) procedure using hydrophobic deep eutectic solvent-based ferrofluid (HDES-FF) as an extractant was established. The developed sample preparation method coupled with high-performance liquid chromatography-diode array detector (HPLC-DAD) was applied to the pretreatment and determination of myclobutanil (MYC) in fruit juice. Hydrophobic deep eutectic solvent, synthesized by n-decanoic acid and DL-menthol, was as a carrier and combined with magnetic nanoparticles (Fe3O4@OA) to form HDES-FF as an extractant with high extraction capacity. The synthesized materials were characterized by Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), and vibrating sample magnetometer (VSM). Parameters affecting extraction efficiency were optimized using single-factor experiments and Box-Behnken design via response surface methodology (BBD-RSM). Parallel tests were performed three times under the optimal conditions predicted by the model, yielding an actual mean recovery of 94.77% with RSD of 2.7% (n = 3) and an enrichment factor of 41.8 ± 0.98 (mean value ± SD, n = 3). Under the optimal conditions, the linear range was 1.0-100.0µg·mL-1; the limit of detection (LOD) and limit of quantification (LOQ) were 0.25 and 0.80µg·mL-1, respectively. The average spiked recoveries in the samples ranged from 98.2 to 100.5% with intra-day relative standard deviations (RSDs) of 1.2-3.5% (n = 3) and inter-day RSDs of 1.1-3.8% (n = 3). Finally, the method was successfully applied to the determination of MYC antimicrobial agent in different fruit juice samples. The proposed HDES-FF-VA-DLLME/HPLC-DAD method was verified to widely apply to the extraction of triazole fungicides.

Hydrophilic interaction liquid chromatography (HILIC) with DAD detection for the determination of relatively non polar fungicides in orange samples

A new, sensitive, rapid, economic and validated high performance liquid chromatography/ diode array detector (HPLC/DAD) method has been developed for the determination of five fungicides namely; Carbendazim (MBC), Thiabendazole (TBZ), Metalaxyl (MET), Imazalil (IMA) and Propiconazole (PCZ). The analytical method was carried on hydrophilic interaction liquid chromatography (HILIC) column using isocratic elution of acetonitrile and water. Prior extraction of orange samples was done using a mixture of diethyl ether and ethyl acetate as an extraction solvent in liquid liquid extraction. The total run time was 15 min which makes it suitable for routine analysis of MBC, TBZ and IMA in oranges. Procedural standard calibration was applied to compensate the matrix effect. In order to measure the lowest concentration of the investigated fungicides below maximum residue limits (MRL), HPLC parameters were optimized. Mean recoveries were obtained ranging from 99.32% to 101.08% with average %RSD < 5.27%. The selected fungicides' residual quantities were successfully measured using the suggested method in various markets and organic orange samples. The investigation of carbendazim's kinetics of degradation, as well as its half-life and predicted preharvest interval (PHI), in real orange samples obtained from orange trees after being treated with the investigated fungicides, is the first to separate relative nonpolar components using HILIC.

Anesthetic Approaches and Perioperative Complications of Total Hip Arthroplasty in Gaucher Disease: A Control-Matched Retrospective-Cohort Study.

Gaucher disease's (GD) pathophysiology generates anesthetic concerns in total hip joint arthroplasty (THA), and due to its rareness, data on perioperative risks are scarce. This 22-year study at a large reference center addresses anesthetic management and perioperative outcomes in GD. This retrospective-cohort study assessed anesthetic success and safety in 30 THA patients, comparing them with a control-matched group. Data on clinical characteristics, perioperative events, and outcomes were collected. The primary outcome was the success rate of anesthesia induction performance at first attempt. Secondary outcomes were difficult intraoperative course and hemodynamic management, and the development of postoperative complications. The age, sex, weight, body mass index, and primary-to-revision hip arthroplasty ratio were similar in both groups. There was no significant difference at all-type anesthesia first initiation attempt success. No particular preference by staff anesthetists for general anesthesia or neuraxial procedures was observed. The GD group showed a significantly higher mean of intraoperative packed Red Blood Cell units administered ((0.73 vs. 0.18); (p = 0.038)), higher intraoperative and postoperative platelet transfusion incidence ((5/30 [16.7%] vs. 0/56 [0.00%]; p = 0.004) and (3/30 [10%] vs. 0/56 [0%]; p = 0.040)), and longer mean recovery room length of stay (426 ± 412 vs. 175 ± 140; p = 0.004). Postoperative complications were not significantly different.

LC-MS/MS Investigation of nitrosamine impurities in certain Sartan group medicinal products available in Istanbul, Türkiye

Nitrosamines (NAs) are molecules that include the nitroso functional group. In 2018, the US Food and Drug Administration (FDA) received its first report of NAs in pharmaceuticals. The fact that NA impurities are likely human carcinogens is relevant to these compounds. Furthermore, prolonged exposure to NA contaminants above safe limits may raise the risk of cancer. The goal of this article was to assess the amounts of six different NAs in Sartan group medicines purchased from formal pharmacies in Istanbul, Türkiye, using a validated LC-MS/MS assay. An LC-MS/MS-based analytical assay was undertaken. The separation was performed with a HR ODS 150mm×3.0mm and 5-analytical columns, providing effective separation of major peaks from NA impurities. In mobile phase A, formic acid was 0.10% in water, while in mobile phase B, formic acid was 0.10% in methanol. The flow rate was 0.4mL/minute, and the total runtime was 18minutes with the gradient elution mode. The validation was conducted in line with ISO/IEC 17025 requirements. Up to 100μg/L, linearity was determined using correlation coefficients (r2>0.995) for all NAs. The limit of quantification values for all NAs analyses were below 1.0μg/L. The mean recovery value obtained during the spike experiment was 95.18%, demonstrating the accuracy of the procedure. In addition, the accuracy was shown by a certified reference analysis, which yielded relative standard deviation and relative error values of 1.82% and 3.34%, respectively. During the intermediate precision testing, bias and relative standard deviation were 0.96 and 2.87%, respectively. Of the 75 study samples involving Sartan group medical products, no nitrosamine impurities were detected, demonstrating that pharmaceutical companies have adequate medication safety precautions in place in accordance with FDA and European Medicines Agency (EMA) regulations published to prevent NA contaminants in human medicinal products.

Comparative cryopreservation of bovine and porcine primary hepatocytes.

The isolation of primary hepatocytes from liver tissue of farm animals yields a very high number of cells, and a part of them can be stored by cryopreservation for future experiments. As no experience exists with the cryopreservation of hepatocytes from cattle, our study aimed at the cryopreservation of bovine hepatocytes by use of different protocols compared with the cryopreservation of hepatocytes from pig. We tested different freezing media (William's Medium E vs. University of Wisconsin solution), cryoprotectants (dimethyl sulfoxide with vs. without trehalose as additional additive), freezing systems (standard freezing container vs. controlled-rate freezer) and freezing times (4 vs. 28 d). These tests identified a general influence of species and freezing systems, whereas the influence of freezing media, trehalose additive and freezing time was less or not obvious. In this regard, we determined a mean recovery of 30% of bovine hepatocytes and 55% of porcine hepatocytes cryopreserved in a controlled-rate freezer, whereas the rates were about 10% less when hepatocytes were frozen in a standard freezing container. In accordance with this observation, the cultivation of cryopreserved hepatocytes from cattle was less effective than that of porcine hepatocytes. Hepatocytes from cattle can be successfully cryopreserved and partially cultured after cryopreservation but with lower percentage than porcine hepatocytes.

Development of highly sensitive relative humidity sensor based on nanoporous PCPDTBT thin film

A novel type of capacitive humidity sensor with surface-type electrode geometry is presented in the present study. The high sensitivity and significantly high bandwidth associated with this planar-type humidity sensor (Al/PCPDTBT/Al) allow the facile and reliable estimation of ambient humidity. The use of a polymer sensing material Poly[2,6-(4,4-bis-(2-ethylhexyl)− 4 H-cyclopenta[2,1-b;3,4-b՛]dithiophene)-alt-4,7(2,1,3-benzothiadiazole)] (PCPDTBT) with hierarchical nanoporous surface morphology and large surface/volume ratio ensures the sensor’s stable performance coupled with swift response to ambient humidity changes. Specifically, at a relatively lower frequency bias signal (i.e., 1 kHz), a fairly higher order of humidity sensitivity has been observed, i.e., 415.07 pF/%RH. While, sensitivities at significantly higher AC signal frequencies (i.e., 10 and 100 kHz) have been experimentally determined to be 345.18 pF/%RH and 154.72 pF/%RH, respectively. Likewise, the resistive sensitivity of the humidity sensor has been estimated to be − 3624.88 kΩ/%RH, − 2381.11 kΩ/%RH and − 1338.14 kΩ/%RH, at 1, 10 and 100 kHz test frequencies, respectively. The operating mechanism of the capacitive humidity sensor relies on an increase in the dielectric constant of the PCPDTBT active sensing layer accompanied by the rise in the ambient humidity levels. In addition to enhanced bandwidth and improved capacitive and resistive sensitivity, the mean response & recovery time of the fabricated device have been recorded to be ∼ 4 min, 17 s and ∼8 min, 43 s, respectively.

Research on artificial neural networks to accurately predict element concentrations in nutrient solutions

Calcium, potassium, nitrogen, magnesium, and phosphorus, the main elements of the nutrient solution, are absorbed by plants and play an important role in plants. By measuring Ca2+, K+, Mg2+, NH4 +, NO3 −, HPO4 2−, the artificial neural networks (ANNs) were used in this study to accurately calculate the concentrations of these elements. Firstly, the error sources of the calculating element concentration were analyzed based on the data of six-ion measurement experiments. Subsequently, various optimization algorithms were compared to optimize back propagation and radial basis function ANNs. Finally, the results of mean relative errors (MREs) and recovery values show that ANNs can effectively reduce the measurement error of ion sensors. From the perspective of recovery values, the prediction error of all elements can be controlled within 15%. From the perspective of MRE, except for magnesium and phosphorus elements, the improved model prediction errors of other elements were also less than 10%.

Coal Fly Ash Modified Graphite-Polyurethane Composite Electrodes for the Electrochemical Determination of Cadmium(II) in Batteries and Water

Coal fly ash (FA), an aluminum silicate by-product and environmental pollutant which is generated during the combustion of coal in coal-fired power stations, was used as an electrode modifier for the determination of Cd(II) in aqueous solutions. In this work, graphite/polyurethane-based composites containing different amounts of FA were prepared and characterized by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX) thermogravimetry (TGA), and derivative thermogravimetry (DTG). The graphite/polyurethane composite electrodes (GPUE), with and without FA modifier, were evaluated with regard to their performance as voltammetric electrodes in the determination of metallic cations, using Cd(II) as a probe. After optimizing solution and instrumental parameters affecting the peak current, a differential pulse anode stripping voltammetry (DPASV) procedure was developed for GPUE modified with 5% FA (m/m), resulting in a linear response for Cd(II) from 2.0 x 10−7 to 1.0 x 10−6 mol L−1 with a detection limit (LOD) of 6.6 x 10−8 mol L−1. Cd(II) was added to natural water samples and determined at the 10−7 mol L−1 level with a mean recovery of 99%. It was also extracted from exhausted rechargeable Ni-Cd batteries and diluted to ca. 0.2 µmol L−1 and determined with the same electrode, with recoveries of 98.7% when compared to FAAS. These results serve as a proof of concept that FA is a useful electrode modifier.

Optimization and validation of an extraction method for the analysis of multi-class emerging contaminants in soil and sediment

Analytical methods for the determination of multi-class emerging contaminants are limited for soil and sediment while they are essential to provide a more complete picture of their distribution in the environment and to understand their fate in different environmental compartments. In this paper, we present the development and optimization of an analytical strategy that combines reliable extraction, purification and the analysis using ultra-pressure liquid chromatography triple quadrupole mass spectrometry (UPLC-MS/MS) of 90 emerging organic contaminants including pesticides, pharmaceuticals and personal care products, flame retardants, per- and polyfluoroalkyl substances (PFASs) and plasticizers in soil and sediment. To extract a wide range of chemicals, the extraction strategy is based on the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) approach. A number of different options were investigated (buffer, acidification, addition of EDTA, different types and combinations of dispersive SPE etc.) and the effectiveness of the chemical extraction procedure and the clean-up was assessed for two matrices: soil (organic matter content of 9%) and sediment (organic matter content of 1.9%). The method was fully validated for both matrices, in terms of accuracy, linearity, repeatability (intra-day), reproducibility (inter-day), method limits of detection and quantification (LODs and MLOQs, respectively). The final performance showed good accuracy and precision (mean recoveries were between 70 and 120% with relative standard deviations (RSD) less than 20% in most cases), low matrix effects, good linearity for the matrix-matched calibration curve (R2≥0.991) and MLOQs ranged from 0.25 and 10 µg/kg. To demonstrate the applicability and suitability of the validated method, soil and sediment samples from Vietnam, France, Sweden and Mexico were analyzed. The results showed that of the 90 target compounds, a total of 33 were quantified in the sediment and soil samples analyzed. In addition to multi-target analysis, this strategy could be suitable for non-target screening, to provide a more comprehensive view of the contaminants present in the samples.

A sensitive LC-MS/MS methotrexate assay capable of assessing adherence to methotrexate therapy in rheumatoid arthritis.

To develop a sensitive liquid chromatography-tandem mass spectrometry method capable of measuring serum methotrexate in patients with rheumatoid arthritis to assess adherence to drug treatment. Isotopically labelled internal standard and deionised water were added to sample prior to solid phase extraction using a Waters Oasis Max ion-exchange 96-well plate. Following extraction, samples were analysed by LC-MS/MS on a TQS-micro mass spectrometer. Mean recovery was 107 % for four different concentrations of methotrexate spiked into seven patient samples, whilst post extraction spiking gave a mean recovery of 100 %. Between-batch and within-batch CVs were≤6 % at three different concentrations of methotrexate in fresh frozen plasma. Mean bias was <5 % for between-batch and within batch analysis at three different weighed in concentrations of methotrexate certified reference material. The lower limit of quantification of the assay was 0.1 nmol/L with linearity up to approximately 100 nmol/L. Dilution linearity studies were used to validate the dilution of patient samples prior to analysis. There was no significant interference in the method from lipaemia, haemolysis or icterus. A sensitive LC-MS/MS assay for methotrexate has been developed and validated. The method has been used to measure methotrexate adherence in patient samples from clinical trials and could be used in future research to assess the ability of the assay as a biofeedback intervention to improve adherence to methotrexate therapy.

Sensitive and rapid quantitation of dexamethasone in human plasma using liquid chromatography coupled with triple quadrupole mass spectrometer.

The aim of this paper was to develop, validate, and utilize a sensitive liquid chromatography-tandem mass spectrometry bioanalytical method for bioequivalence/clinical trial studies conducted in human plasma. To accomplish the target, a stable labeled internal standard, that is, dexamethasone D4 was used as an internal standard to track and compensate the parent compound during processing, and extraction from plasma. The method involves a rapid liquid-liquid phase extraction from plasma, followed by reverse phase chromatography, and mass spectrometry detection, with a total run time of 3.5 min. The method was developed and validated from 2 to 600 ng/ml for dexamethasone. The mean recovery for dexamethasone was found to be 81.0%. The validated method enabled the analysis of dexamethasone in samples from clinical pharmacokinetic studies. The peak concentration of dexamethasone ranged between 253 to 281 ng/ml and 319 to 343 ng/ml, respectively, in fasted and fed conditions. The terminal half-life values for dexamethasone ranged between 3.5 to 8.2 h and 3.0 to 7.5 h, respectively.

Development and validation of a rapid and sensitive LC-MS/MS approach for alkaloid testing in different Lupinus species

Foods derived from lupin are attracting consumers and producers for their nutritional value and low cost of production. Lupin products may pose a health risk to consumers due to the presence of toxic alkaloid compounds. To monitor alkaloids in lupin seeds, we developed and validated a rapid LC-MS/MS method for the determination of five quinolizidine alkaloids and one indole alkaloid in lupin seeds. The final method involves extraction by water/acetonitrile, ultrasonication, separation using NaCl and MgSO4, alkalinisation by NaOH and analysis using HPLC-MS/MS. The separation was achieved in 6 min using HPLC directly coupled to MS/MS on a 6500 + QTRAP in ESI-positive mode. The method showed acceptable recovery for all tested compounds in soybean grain at a wide range from 0.55 (LOQ) to 55 mg/kg, with a mean recovery of 93% for the total alkaloid content (SD <2.5%). The method was tested on a commercial lupin flour sample yielding an alkaloid concentration of 130 mg/kg (SD 3.6%). Alkaloid profiles were assessed across different cultivars of five Lupinus species (Lupinus angustifolius, L. cosentinii, L. albus, L. luteus, and L. mutabilis). Using the method presented, toxic alkaloid levels can be monitored in lupin-based products to ensure their safety for human consumption. The method was deployed to measure the alkaloid content across different seeds of narrow-leaf lupin from the same farm, revealing that the alkaloid content varied widely from seed to seed from the same farm.

LC-MS/MS-MS3 for the Determination and Quantification of Δ9-Tetrahydrocannabinol and Metabolites in Blood Samples.

Due to the high prevalence of cannabinoids in forensic toxicology analysis, it is crucial to have an efficient method that allows the use of a small sample amount and that requires a minimal sample preparation, for the determination and quantification of low concentrations. A simple, highly selective and high throughput liquid chromatography tandem mass spectrometry methodology (LC-MS/MS-MS3) was developed for the determination and quantification of ∆9-tetrahydrocannabinol (THC), 11-hydroxy-∆9- tetrahydrocannabinol (THC-OH) and 11-nor-9-carboxy-∆9-tetrahydrocannabinol (THC-COOH), in blood samples. Chromatographic analysis of THC, THC-OH, and THC-COOH and their deuterated internal standards was preceded by protein precipitation (PPT) of 0.1 mL of blood samples with acetonitrile. Chromatographic separation was achieved by use of an Acquity UPLC® HHS T3 (100 mm x 2.1mm i.d., 1.8 μm) reversed-phase column, using a gradient elution of 2 mM aqueous ammonium formate, 0.1% formic acid, and methanol at a flow rate of 0.4 mL/min, with a run time of 10 minutes. For the MS/MS-MS3 analysis, a SCIEX QTRAP® 6500+ triple quadrupole linear ion trap mass spectrometer was used via electrospray ionization (ESI), operated in multiple reaction monitoring (MRM) and linear ion trap mode (MS3). The method was validated in accordance with internationally accepted criteria and guidelines, and proved to be selective and linear between 0.5-100 ng/mL (r2>0.995). The lower limits of quantification (LLOQ) corresponded to the lowest concentrations used for the calibration curves. The coefficients of variation obtained for accuracy and precision were <15%. The mean recoveries were between 88.0-117.2%, for the studied concentration levels (1 ng/mL, 5 ng/mL and 50 ng/mL). No significant interfering compounds, matrix effects or carryover were observed. The validated method provides a sensitive, efficient and robust procedure for the quantification of cannabinoids in blood, using LC-MS/MS-MS3 and a sample volume of 0.1 mL. This work is also a proof of concept for using LC-MS3 technique to determine drugs in biological samples.

Latent heat recovery of composite PCM for hybrid BTMSs based on micro-encapsulated phase change slurry

Phase change material (PCM) cooling is widely applied in battery thermal management systems (BTMS) due to high latent heat. To address the long latent heat recovery time of PCM, especially in continuous discharge and charge cycles, a novel hybrid BTMS coupling dual-PCM is designed. The dual-PCM contains the composite PCM as the main heat dissipation and the micro-encapsulated phase change slurry (MEPCS) for latent heat recovery. The experiments are performed to ensure the effectiveness of the hybrid BTMS. The temperature performance of the battery module, solidification rate of composite PCM and pressure drop of the MEPCS are studied as the critical performance indicators. To establish a trade-off between these performance indicators, the interaction effects between inlet velocities and mass concentrations of the MEPCS are investigated. Meanwhile, different ambient temperatures combined with mass concentrations are considered. Results indicate that MEPCS as the coolant has a significant effect on the temperature and solidification performances at low inlet velocity. The higher mass concentration of MEPCS does not mean better heat recovery capacity at the same pressure drop. Considering the fluctuation of the solidification performance, the mass concentration of MEPCS above 10 % is recommended to meet the challenges of different ambient temperatures. The energy efficiency is optimized by adjusting the mass concentration and inlet velocity. The maximum reduction in pressure drop is 39.8 % with high temperature and solidification performances. The solutions can reduce energy consumption and improve the economic benefits for BTMS.

Simultaneous Determination of Multiple Contaminants in Chicken Liver Using Dispersive Liquid-Liquid Microextraction (DLLME) Detected by LC-HRMS/MS

Simultaneous determination of a mixture of food contaminants, including pesticides, sulphonamides, fluoroquinolones, anthelmintics, and aflatoxin B1, in solid biological samples (chicken liver) by dispersive liquid-liquid microextraction/liquid chromatography-high resolution mass spectrometry (DLLME/LC-HRMS) is presented. Previous work focused on the application of DLLME to single-class contaminants. In this work, the DLLME extraction method has been extended to complex multiresidues in the biological matrix. The first part of this study was the selection of an appropriate solvent that enabled the dissolution of analytes from the chicken livers. The matrix-matched calibration curves showed good linearity in the range 0.5–50.0 µg kg−1 for aflatoxin B1 and 50–500 µg kg−1 for pesticides, fluoroquinolones, sulphonamides, and anthelmintics, with a coefficient of determination (R2) values of 0.9916–0.9967. The mean recoveries were in the range of 80.4–96.3%, and the relative standard deviation (RSD) values were in the range of 1.53–8.98%. The limit of detection (LOD) and the limit of quantification (LOQ) values were 0.03 µg kg−1 and 0.09 µg kg−1, respectively, for aflatoxin B1, and for pesticides, fluoroquinolones, sulphonamides, and anthelmintics, they were in the range of 0.011–1.197 µg kg−1 and 0.150–2.579 µg kg−1, respectively. The developed method was compared with the standard solid phase extraction (SPE) method, and there was no significant difference between the two methods.

Analytical Method Development and Validation of Ornidazole in Bulk and Dosage Form

Abstract: In the given study, of an For the purpose of estimating ornidazole in bulk and dose form, an correct, exact, and specific approach has been established. by ultraviolet spectroscopy. Ornidazole belongs to the categories of antibacterial medications ( nitroimidazoles) also used to treat infections caused by anaerobic bacteria and protozoa. The procedure includes calculation of the absorbance of Ornidazole blend in Methanol water 1:9. The calibration curve method shows wavelength maxima for Ornidazole at 315 nm with Methanol water 1:9 in the wavelength having a correlation value of 0.999, between 2-28 g/ml. The mean recovery of Ornidazole was discovered to be in pharmaceutical dosage form 95.5%. Results of experiments were authenticated for Accuracy: correctness, exactness, precision, truthfulness, reliability, validity established adequately. The submission process is easy, quick, and appropriate for standard analysis. Statistics were used to validate the analysis' findings, and recovery studies were administered as per the guidelines of ICH.

Evaluation of the derivative spectrophotometric technique for the quantification of ofloxacin and ciprofloxacin hydrochloride in their bulk drugs and pharmaceutical dosage forms

It was developed and validated as a sensitive, economical, and repeatable derivative visible-spectrophotometric method for determining ciprofloxacin hydrochloride and ofloxacin. The first, second, third, and fourth derivative spectra of the standard solutions were obtained by instrumental electronic differentiation with a delta lambda (Δλ) of 8 nm, and the spectra of the solutions were recorded in the range of 250–350 nm. The distances between the center zero baselines and the 280 nm negative peak were used to measure the analytical responses. The developed method achieves a low detection limit of 0.3 μg/L with a linear range of 2–20 μg/L. with a good precision (RSD ≤ 2.0%) The developed method is sensitive and precise. simple, accurate, and cost-effective, and exhibited a good correlation coefficient (R2 = 0.9998) and excellent mean recovery (99.20–100.08%), indicating a high degree of precision of the methods. The method's accuracy, precision, selectivity, robustness, and linearity were all demonstrated via a rigorous verification process in compliance with ICH guidelines. The recommended method may be used to control the quality of dosages that contain ofloxacien and ciprofloxacin hydrochloride as an active component since it is easy, inexpensive, and reliable enough.