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Journal of Pharmaceutical and... Sep 2023A new, reversed-phase HPLC (RP-HPLC) method was developed for the simultaneous determination of the dipeptidyl-peptidase-IV-inhibitor antidiabetic drug vildagliptin...
Simultaneous determination of enantiomeric and organic impurities of vildagliptin on a cellulose tris(3-chloro-4-methylphenylcarbamate) column under revered-phase conditions.
A new, reversed-phase HPLC (RP-HPLC) method was developed for the simultaneous determination of the dipeptidyl-peptidase-IV-inhibitor antidiabetic drug vildagliptin (VIL) enantiomeric impurity and four other achiral related impurities. An initial screening was performed on five polysaccharide-type chiral stationary phases (Lux Amylose-1, Lux Amylose-2, Lux-Cellulose-1, Lux-Cellulose-2, Lux-Cellulose-3) in polar organic mode with methanol, ethanol, 2-propanol, or acetonitrile containing 0,1% diethylamine as mobile phase to identify the best conditions for the separation of VIL enantiomers. Lux-Cellulose-2 column was found to provide the best chiral resolution for VIL enantiomers. Further experiments were conducted using different aqueous-organic mobile phases to achieve the simultaneous chiral-achiral separation of the selected compounds. Experimental design-based optimization was performed by using a face-centered central composite design. The optimal separation conditions (Lux Cellulose-2 stationary phase, 45 °C, mobile phase consisting of methanol/water/diethylamine 80:20:0.2 (v/v/v), and 0.45 mL/min flow rate) provided baseline separation for all 6 compounds. The optimized method was validated according to the ICH guideline and proved to be reliable, specific, linear, precise, and accurate for the determination of at least 0.1% for all impurities in VIL samples. The validated method was applied for determinations from a commercially available drug formulation and proved to be suitable for routine quality control of both enantiomeric and organic impurities of VIL.
Topics: Amylose; Vildagliptin; Methanol; Cellulose; Chromatography, High Pressure Liquid; Water; Stereoisomerism
PubMed: 37343452
DOI: 10.1016/j.jpba.2023.115495 -
Biomedical Chromatography : BMC Nov 2023Glipizide is an antidiabetic drug used for the treatment of type 2 diabetes. A simple, reliable and robust reverse-phase liquid chromatographic method (RP-HPLC) was...
Stability-indicating method development and validation for quantitative estimation of organic impurities of the antidiabetic drug glipizide in drug substance and pharmaceutical dosage form using HPLC.
Glipizide is an antidiabetic drug used for the treatment of type 2 diabetes. A simple, reliable and robust reverse-phase liquid chromatographic method (RP-HPLC) was developed and validated as per International Conference on Harmonization Q2(R1) for estimating the impurities of glipizide in pharmaceutical formulations. The chromatographic separation was carried out on a Phenomenex Luna C (2) 250 × 4.6 mm, 5 μm with a binary solvent delivery system [MP-A, a homogenous mixture of water and acetonitrile in a ratio of 90:10 (v/v) and 1 ml of orthophosphoric acid; and MP-B, a homogenous mixture of water and acetonitrile in a ratio of 10:90 (v/v) and 1 ml of orthophosphoric acid] with a detection wavelength of 225 nm, a column temperature of 30°C, a flow rate of 1.5 ml/min, and an injection volume of 20 μl. All process, degradant and unknown impurities were separated well with a resolution >2.2 and were estimated accurately without any interference. The recovered values and regression values were 98.7-100.5% and R > 0.9999, respectively. The recovery and linearity studies covered the quantitation limit to 150% of the specification limit. The stability-indicating properties of the developed RP-HPLC method was assessed from the forced degradation studies. The developed method was successfully applied for real-time sample analysis of the glipizide dosage form.
PubMed: 37635093
DOI: 10.1002/bmc.5727 -
Yakugaku Zasshi : Journal of the... 2024Crude drugs and Kampo formulations derived from natural materials such as plants, animals, and minerals are multicomponent medicines that contain numerous chemical... (Review)
Review
Crude drugs and Kampo formulations derived from natural materials such as plants, animals, and minerals are multicomponent medicines that contain numerous chemical constituents. Quantitative determination of characteristic constituents for quality control is crucial for the standardization and quality assurance of natural medicines. Quantitative assays to determine marker compound contents are commonly performed using HPLC systems. In order to achieve accurate quantitative determination, it is essential to use standard materials with well-defined purities corresponding to the target analytes. Many marker compounds used as standard materials must be purified and isolated from natural products while ensuring sufficient purity. However, the composition of impurities in the standard material differs among different batches due to differences in the raw materials and their extraction, separation, and purification processes. Therefore, controlling the purity of standard materials derived from natural products is more complex than that of synthetic substances. Quantitative NMR (qNMR), which has become widely used as an absolute quantitative method for low-molecule organic compounds, makes it possible to solve these issues. qNMR has been introduced into the crude drug section of the Japanese Pharmacopoeia (JP) for evaluating the purity of standard materials used for the assay. This review outlines an example of quantitative determination using relative molar sensitivity (RMS) based on qNMR adopted in the JP and introduces the latest efforts toward the application of qNMR to standard materials used for crude drugs in this context.
Topics: Magnetic Resonance Spectroscopy; Quality Control; Biological Products; Chromatography, High Pressure Liquid; Medicine, Kampo
PubMed: 38556310
DOI: 10.1248/yakushi.23-00151-5 -
BMC Chemistry Jan 2024Bromhexine (BR), guaiafenesin (GUF) and salbutamol (SAL) are formulated as Ventocough syrup® (with and without sugar), labeled to contain propyl paraben and sodium...
Bromhexine (BR), guaiafenesin (GUF) and salbutamol (SAL) are formulated as Ventocough syrup® (with and without sugar), labeled to contain propyl paraben and sodium benzoate as inactive ingredients. They are used to make coughing more productive and easier. A crucial element and a major issue in the pharmaceutical industry is the control of organic related impurities to obtain safe and effective treatment. Guaiacol (GUL) is reported to be GUF related impurity that was proved to be extremely toxic (toxic rating class 5), and its use should be banned. In this work, In-Silico study and ADMET estimation were conducted to predict GUL pharmacokinetic properties and its toxicity profile. Additionally, two chromatographic methods were conducted to analyze the studied components along with GUF impurity in the presence of the labeled dosage form excipients. The In-Silico study assured that GUL has oral rat acute toxicity and it is considered to be skin sensitizer. On the other hand, the developed TLC- densitometeric method depended on using a mobile phase mixture of hexane: methylene chloride: triethylamine (5.0:6.0:0.3, by volume) as a developing system. UV-Scanning was performed immediately at 275 nm for SAL, GUF and GUL, while scanning at 310 nm was used for scanning BR. Linearity was established in the ranges of 0.25-4.0, 0.25-4.0, 0.5-8.0 and 0.1-1.6 µg/band for BR, SAL, GUF and GUL, respectively. In the developed HPLC method, separation was performed on X-Bridge® C column (250 × 4.6 mm, 5 μm) using a solvent mixture of 0.05M disodium hydrogen phosphate pH 3 with aqueous phosphoric acid: methanol (containing 0.3%, v/v triethylamine) (40:60, v/v). Detection was done at 225 nm and separation was achieved within 10 min. Linearity was proved in the range of 2-50 µg/mL for the proposed drugs. Validation of the developed methods was done and all the calculated parameters were within the acceptable limits recommended by ICH guidelines. After that, methods were used to examine the potency of the selected marketed dosage forms and concentrations of all drugs were within the acceptable limits. Additionally, complete separation between the studied drugs and the additives were observed. The developed methods can be used during routine quality control analysis of the proposed drugs when the required issues concern on sensitivity, selectivity and analysis time.
PubMed: 38281055
DOI: 10.1186/s13065-024-01122-5 -
Science Advances Sep 2023Saturated fatty acids are abundant organic compounds in oceans and sea sprays. Their photochemical reactions induced by solar radiation have recently been found as an...
Saturated fatty acids are abundant organic compounds in oceans and sea sprays. Their photochemical reactions induced by solar radiation have recently been found as an abiotic source of volatile organic compounds, which serve as precursors of secondary organic aerosols. However, photoabsorption of wavelengths longer than 250 nanometers in liquid saturated fatty acids remains unexplained, despite being first reported in 1931. Here, we demonstrate that the previously reported absorption of wavelengths longer than 250 nanometers by liquid nonanoic acid [CH(CH)COOH)] originates from traces of impurities (0.1% at most) intrinsically contained in nonanoic acid reagents. Absorption cross sections of nonanoic acid newly obtained here indicate that the upper limit of its photolysis rate is three to five orders of magnitude smaller than those for atmospherically relevant carbonyl compounds.
PubMed: 37729407
DOI: 10.1126/sciadv.adj6438 -
Environmental Monitoring and Assessment Jan 2024Water pollution stands as a critical worldwide concern, bearing extensive repercussions that extend to human health and the natural ecosystem. The sources of water... (Review)
Review
Water pollution stands as a critical worldwide concern, bearing extensive repercussions that extend to human health and the natural ecosystem. The sources of water pollution can be diverse, arising from natural processes and human activities and the pollutants may range from chemical and biological agents to physical and radiological contaminants. The contamination of water disrupts the natural functioning of the system, leading to both immediate and prolonged health problems. Various technologies and procedures, ranging from conventional to advanced, have been developed to eliminate water impurities, with the choice depending on the type and level of contamination. Assessing risks is a crucial element in guaranteeing the safety of drinking water. Till now, research is continuing the removal of contaminates for the sake of supplying safe drinking water. The study examined physical, inorganic, organic, biological and radiological contaminants in drinking water. It looked at where these contaminants come from, their characteristics, the impact they have and successful methods used in real-world situations to clean the contaminated water. Risk assessment methodologies associated with the use of unsafe drinking water as future directives are also taken into consideration in the present study for the benefit of public concern. The manuscript introduces a comprehensive study on water pollution, focusing on assessing and mitigating risks associated with physical, inorganic, organic, biological and radiological contaminants in drinking water, with a novel emphasis on future directives and sustainable solutions for public safety.
Topics: Humans; Drinking Water; Ecosystem; Environmental Monitoring; Water Supply; Risk Assessment; Water Pollutants, Chemical
PubMed: 38244090
DOI: 10.1007/s10661-024-12311-z -
Foods (Basel, Switzerland) Aug 2023Wei safflower seed oil (WSO) prepared by the cold pressing method and organic solvent extraction method was characterized in this study. The yield of cold-pressed WSO...
Wei safflower seed oil (WSO) prepared by the cold pressing method and organic solvent extraction method was characterized in this study. The yield of cold-pressed WSO (CP-WSO) was inferior to that of -hexane-extracted WSO (HE-WSO). The physicochemical properties (refractive index, density, iodine value, insoluble impurities) and fatty acid compositions were similar, and both were rich in linoleic acid. However, CP-WSO had better color and less solvent residue. The type and content of vitamin E in CP-WSO was also superior to that in HE-WSO, which explained the high oxidative stability of CP-WSO in the Rancimat test. Our results provide a reference for the development of Wei safflower seed oil.
PubMed: 37685161
DOI: 10.3390/foods12173228 -
Biotechnology Progress 2024In the production of biological therapeutics such as monoclonal antibodies (mAbs), ultrafiltration and diafiltration (UF/DF) are widely regarded as effective downstream...
In the production of biological therapeutics such as monoclonal antibodies (mAbs), ultrafiltration and diafiltration (UF/DF) are widely regarded as effective downstream processing steps capable of removing process equipment related leachables (PERLs) introduced upstream of the UF/DF step. However, clearance data available in the literature are limited to species with low partition coefficients (log P) such as buffer ions, hydrophilic organic compounds, and some metal ions. Additional data for a wide range of PERLs including hydrophobic compounds and elemental impurities are needed to establish meaningful, comprehensive safety risk assessments. Herein, we report the results from studies investigating the clearance of seven different organic PERLs representing a wide range of characteristics (i.e., log P (-0.3 to 18)), and four model elements with different chemical properties spiked into a mAb formulation at 10 ppm and analyzed during clearance using gas chromatography-mass spectrometry (GC-MS), liquid chromatography-photodiode-array-mass spectrometry (LC-PDA-MS), and inductively coupled plasma mass spectrometry (ICP-MS). The clearance data showed ideal clearance and sieving of spiked organic PERLs with log P < 4, partial clearance of PERLs with 4 < log P < 9, and poor clearance of highly hydrophobic PERLs (log P > 9) after nine diafiltration volumes (DVs). Supplemental clearance studies on seven additional PERLs present at much lower concentration levels (0.1-1.5 ppm) in the mAb formulation upstream of UF/DF and three PERLs associated with the tangential flow filtration (TFF) equipment also demonstrated the similar correlations between log P and % clearance. For model elements, the findings suggest that UF/DF in general provides ideal clearance for elements. Evidence showed that the UF/DF process does not only help mitigate leachables risk from PERLs introduced upstream of UF/DF, but also from the TFF operation itself as all three TFF-related PERLs were effectively cleared. Overall, the UF/DF clearance presented in this work demonstrated whereas highly hydrophobic PERLs and elements that exist as charged species, particularly transition metal ions, may not be as effectively cleared and thus warrant further risk assessment; hydrophilic and some hydrophobic PERLs (log P < 4) are indeed well-cleared and thus present a lower overall safety risk.
Topics: Ultrafiltration; Filtration; Organic Chemicals; Ions
PubMed: 37964726
DOI: 10.1002/btpr.3400 -
Advanced Science (Weinheim,... Jan 2024Metal-organic frameworks (MOFs) have played a crucial role in recent advancements in developing lithium-based battery electrolytes, electrodes, and separators. Although... (Review)
Review
Metal-organic frameworks (MOFs) have played a crucial role in recent advancements in developing lithium-based battery electrolytes, electrodes, and separators. Although many MOF-based battery components rely on their well-defined porosity and controllable functionality, they also boast a myriad of other significant properties relevant to battery applications. In this mini-review, the distinct advantages of MOFs in battery applications are discussed, including using MOFs to 1) scavenge impurities to increase cycling stability, 2) widen the operation temperature range of conventional electrolytes, 3) widen the operation voltage range of common electrolytes, and 4) employ as artificial solid-electrolyte interphases to prevent lithium dendrite growth. Furthermore, subsisting challenges of developing these emerging MOF-based battery technologies are discussed and guidance for shaping the future of this field is given.
PubMed: 37946699
DOI: 10.1002/advs.202305280 -
The Science of the Total Environment Oct 2023The abilities of improving phosphorus (P) resources sustainability and reducing water eutrophication make struvite crystallization technology attract increasing interest...
The abilities of improving phosphorus (P) resources sustainability and reducing water eutrophication make struvite crystallization technology attract increasing interest in wastewater treatment, but struvite crystallization process may be affected by various impurities in wastewater. In this study, the effects of nine representative ionic surfactants including three types (anionic, cationic and zwitterionic) on crystallization kinetics and product quality of struvite were investigated, and the influencing mechanism was further probed. The results demonstrated that anionic surfactants significantly inhibit crystal growth so as to reduce crystal size especially in a-axis direction, change crystal morphology and decrease P recovery efficiency, and also lead to a slight decline in product purity. In contrast, cationic and zwitterionic surfactants have no obvious influence on the formation of struvite. A series of experimental characterizations and molecular simulations collectively revealed that the inhibition of crystal growth by anionic surfactants is attributed to the adsorption of anionic surfactant molecules on struvite crystal surface and subsequent blockage of active growth sites. The binding ability of surfactant molecules with the Mg exposed on struvite crystal surface was highlighted to be the most essential factor determining the adsorption behavior and adsorption capacity. Anionic surfactants with stronger binding ability with Mg have more intense inhibitory effect, but a large molecular volume of anionic surfactants will weaken the adsorption capacity on crystal surface so as to reduce the inhibitory effect. Contrastively, cationic and zwitterion surfactants without binding ability with Mg have no inhibitory effect. These findings enable us to have a clearer understanding of the impact of organic pollutants on struvite crystallization and make a preliminary judgment on the organic pollutants that may have the ability to inhibit the crystal growth of struvite.
PubMed: 37329921
DOI: 10.1016/j.scitotenv.2023.164882