High‐performance LiFePO 4 cathode material was prepared by multiple intensification process with acid‐washed iron red as raw material

Author(s):  
Qing Wang ◽  
Yafeng Wang ◽  
Shao‐hua Luo ◽  
Pengwei Li ◽  
Shengxue Yan ◽  
...  
Author(s):  
Firmansyah A. ◽  
Winingsih W. ◽  
Soebara Y S

Analysis of natural product remain challenging issues for analytical chemist, since natural products are complicated system of mixture. The most popular methods of choice used for quality control of raw material and finished product are high performance liquid chromatography (HPLC), gas chromatography (GC) and mass spectrometry (MS). The utilization of FTIR-ATR (Fourier Transform Infrared-Attenuated Total Reflectance) method in natural product analysis is still limited. This study attempts to expand the use of FTIR spectroscopy in authenticating Indonesian coffee powder.The coffee samples studied were taken from nine regions in Indonesia, namely Aceh Gayo, Flores, Kintamani, Mandheling, Papua, Sidikalang, Toraja, Kerinci and Lampung.The samples in the form of coffee bean from various regions were powdered . The next step conducted was to determine the spectrum using the FTIR-ATR (Attenuated Total Reflectance) using ZnSe crystal of 8000 resolution. Spectrum samples, then, were analyzed using chemometrics. The utilized chemometric model was the principal component analysis (PCA) and cluster analysis (CA). Based on the chemometric analysis, there are similarities between Aceh Gayo coffee with Toraja coffee, Mandailing coffee, Kintamani coffee and Flores coffee. Sidikalang coffee has a similarity to Flores coffee; Papua coffee has a similarity to Sidikalang coffee; Lampung coffee has a similarity to Sidikalang coffee, while Kerinci coffee has a similarity to Papua coffee.


2019 ◽  
Vol 16 ◽  
Author(s):  
Joanna Wittckind Manoel ◽  
Camila Ferrazza Alves Giordani ◽  
Livia Maronesi Bueno ◽  
Sarah Chagas Campanharo ◽  
Elfrides Eva Sherman Schapoval ◽  
...  

Introduction: Impurity analysis is an important step in the quality control of pharmaceutical ingredients and final product. Impurities can arise from drug synthesis or excipients and even at small concentrations may affect product efficacy and safety. In this work two methods using high performance liquid chromatography (HPLC) were developed and validated for the evaluation of besifloxacin and its impurity synthesis, with isocratic elution and another with gradient elution. Method: The analysis by HPLC in isocratic elution mode was performed using a cyano column maintained at 25 °C. The mobile phase was composed by 0.5% triethylamine (pH 3.0): acetonitrile (88:12 v/v) eluted at a flow rate of 1.0 ml/min with detection at 330 nm. The gradient elution method was carried out with the same column and mobile phase components only modifying the rate between organic and aqueous phase during analysis. The procedures have been validated according to internationally accepted guidelines, observing results within acceptable limits. Results: The methods presented were found to be linear in the 140 to 260 µg/ml range for besifloxacin and 0.3 to 2.3 µg/ml for an impurity named A. The limits of detection and quantification were respectively 0.07 and 0.3 µg/ml for impurity A, with a 20 µL injection volume. The precision achieved for all analyses performed provided RSD inter-day equal to 6.47 and 6.36% for impurity A with isocratic elution and gradient, respectively. The accuracy was higher than 99% and robustness exhibited satisfactory results. In the isocratic method an analysis time of 25 min and 15 min was obtained for gradient. For impurity A, the number of theoretical plates in the isocratic mode was about 5000 while in the gradient mode it was about 45000, hence, it made the column more efficient by changing the mobile phase composition during elution. In besifloxacin raw material and in pharmaceutical product used in this study, other related impurities were present but but impurity A was searched for and not detected Conclusion: The proposed methods can be applied for quantitative determination of impurities in the analysis of the besifloxacin raw material, as well as in ophthalmic suspension of the drug, considering the quantitation limit.


2021 ◽  
Vol 5 (6) ◽  
pp. 151
Author(s):  
Mustapha El Kanzaoui ◽  
Chouaib Ennawaoui ◽  
Saleh Eladaoui ◽  
Abdelowahed Hajjaji ◽  
Abdellah Guenbour ◽  
...  

Given the amount of industrial waste produced and collected in the world today, a recycling and recovery process is needed. The study carried out on this subject focuses on the valorization of one of these industrial wastes, namely the fly ash produced by an ultra-supercritical coal power plant. This paper describes the use and recovery of fly ash as a high percentage reinforcement for the development of a new high-performance composite material for use in various fields. The raw material, fly ash, comes from the staged combustion of coal, which occurs in the furnace of an ultra-supercritical boiler of a coal-fired power plant. Mechanical compression, thermal conductivity, and erosion tests are used to study the mechanical, thermal, and erosion behavior of this new composite material. The mineralogical and textural analyses of samples were characterized using Scanning Electron Microscopy (SEM). SEM confirmed the formation of a new composite by a polymerization reaction. The results obtained are very remarkable, with a high Young’s modulus and a criterion of insulation, which approves the presence of a potential to be exploited in the different fields of materials. In conclusion, the composite material presented in this study has great potential for building material and could represent interesting candidates for the smart city.


2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Min Kyoung Kim ◽  
Sang Cheol Park ◽  
Geonha Park ◽  
Eunjung Choi ◽  
Yura Ji ◽  
...  

AbstractThe present study introduces a systematic approach using analytical quality by design (AQbD) methodology for the development of a qualified liquid chromatographic analytical method, which is a challenge in herbal medicinal products due to the intrinsic complex components of botanical sources. The ultra-high-performance liquid chromatography-photodiode array-mass spectrometry (UHPLC-PDA-MS) technique for 11 flavonoids in Genkwa Flos was utilized through the entire analytical processes, from the risk assessment study to the factor screening test, and finally in method optimization employing central composite design (CCD). In this approach, column temperature and mobile solvent slope were found to be critical method parameters (CMPs) and each of the eleven flavonoid peaks’ resolution values were used as critical method attributes (CMAs) through data mining conversion formulas. An optimum chromatographic method in the design space was calculated by mathematical and response surface methodology (RSM). The established chromatographic condition is as follows: acetonitrile and 0.1% formic acid gradient elution (0–13 min, 10–45%; 13–13.5 min, 45–100%; 13.5–14 min, 100–10%; 14–15 min, 10% acetonitrile), column temperature 28℃, detection wavelength 335 nm, and flow rate 0.35 mL/min using C18 (50 × 2.1 mm, 1.7 μm) column. A validation study was also performed successfully for apigenin 7-O-glucuronide, apigenin, and genkwanin. A few important validation results were as follows: linearity over 0.999 coefficient of correlation, detection limit of 2.87–22.41, quantitation limit of 8.70–67.92, relative standard deviation of precision less than 0.22%, and accuracy between 100.13 and 102.49% for apigenin, genkwanin, and apigenin 7-O-glucuronide. In conclusion, the present design-based approach provide a systematic platform that can be effectively applied to ensure pharmaceutically qualified analytical data from complex natural products based botanical drug.


2021 ◽  
Vol 14 (4) ◽  
pp. 310
Author(s):  
Ana V. González-de-Peredo ◽  
Mercedes Vázquez-Espinosa ◽  
Ceferino Carrera ◽  
Estrella Espada-Bellido ◽  
Marta Ferreiro-González ◽  
...  

Onion, one of the most consumed vegetables in the world, is also known to contain high levels of antioxidant compounds, with protective effects against different degenerative pathologies. Specifically, onion is rich in flavonols, mainly quercetin derivatives, which are compounds with high antioxidant and free radical scavenging power. For this reason, it is of the utmost importance to count on optimal analytical methods that allow for the determination and quantification of these compounds of interest. A rapid ultra-high performance liquid chromatography (UHPLC)-photo-diode array (PDA) method for the separation of the major flavonols in onions was developed using a Box–Behnken design in conjunction with multiresponse optimization on the basis of the desirability function. The conditions that provided a successful separation were 9.9% and 53.2% of phase B at the beginning and at the end of the gradient, respectively; 55 °C column working temperature; and 0.6 mL min−1 flow rate. The complete separation was achieved in less than 2.7 min with excellent chromatographic characteristics. The method was validated, and its high precision, low detection and quantification limits, good linearity, and robustness were confirmed. The correct applicability of the method improves the analysis of the raw material, increasing the quality of onions and its subproducts in terms of bioactive compounds and functional characteristics for consumers.


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