scholarly journals Extraction Procedure Optimization of Atenolol from Dried Plasma Spots

Author(s):  
A. A. Chernonosov ◽  
V. V. Koval

Aims: Atenolol is one of the β-blockers widely used for the treatment of hypertension and other cardiovascular diseases. To simplify the methods for determining of drugs concentrations in blood and plasma the dried spots assays (dried blood spots or dried plasma spots) could be used. In this case high sensitive detector like mass-spectrometer is required as well as high level of drug recovery from dried spot. In this study the extraction of atenolol from dried plasma spots (DPS) was studied to offer the optimum parameters of extraction method. Study Design: Short research articles. Place and Duration of Study: Core Facility of Mass Spectrometric Analysis, Institute of Chemical Biology and Fundamental Medicine SB RAS, between January and October 2019. Methodology: The organic extraction method was chosen for evaluation as the most suitable for LC-MS assay. Several parameters: % of organic solvent, presence or absence of 0.1% formic acid, time, volume and temperature of extraction were investigated to find the best combination for atenolol recovery from DPS for further LC-MS analysis. Results: Results showed that the solvent composition and temperature has main influence on the extraction. The effect of extraction time and volume of solvent have no significant influence on atenolol recovery. Pure acetonitrile is the worst solvent for atenolol extraction from DPS. The solvents: MeOH:H2O (60:40, v:v), MeOH:0.1% FA in H2O (60:40, v:v), ACN:0.1% FA in H2O (50:50, v:v) or ACN:MeOH (60:40, v:v) provide the best recovery of atenolol . The optimum extraction temperature is 40°C, time of extraction is 15-30 min and volume of solvent - 200-300 μL. Conclusion: Several solvents acceptable for LC-MS analysis with optimized recovery parameter from DPS can be used for routine extraction of atenolol.

Author(s):  
L. V. Aksenova ◽  
V. V. Koval ◽  
A. A. Chernonosov

Aims: Apixaban is an anticoagulant used to treat and prevent blood clots, as well as to prevent stroke in people with atrial fibrillation. The dried spot analyses, including dried blood spots and dried plasma spots, are used to simplify techniques for determining drug concentrations in blood and plasma. In this case, equipment with highly sensitive detector is required, for example, mass spectrometer, as well as a high level of drug extraction from the dried spot. In this work, apixaban extraction from dried plasma spots (DPS) was studied in order to determine the optimal parameters of the extraction method. Study Design: Short Research Articles. Place and Duration of Study: Core Facility of Mass Spectrometric Analysis, Institute of Chemical Biology and Fundamental Medicine SB RAS, between September 2019 and February 2020. Methodology: The organic extraction method was chosen for evaluation as the most suitable for LC-MS assay. Several parameters: percentage of organic solvent, presence or absence of 0.1% formic acid (FA), time, volume and temperature of extraction were investigated to find the best combination for recovery of apixaban from DPS for further LC-MS analysis. Results: The results showed that the main influence on the extraction is the composition of the solvent, volume of solvent, as well as temperature and time of extraction. Pure acetonitrile is the worst solvent for extracting apixaban from DPS. Solvents: MeOH:H2O (100:0, v: v), MeOH: 0.1% FA in H2O (80:20, v:v), ACN: 0.1% FA in H2O (90:10, v:v) or ACN:MeOH (90:10, v:v) provide better recovery of apixaban. The optimum extraction parameters were as follows: 90% acetonitrile concentration, extraction temperature of 40°C, extraction time of 15 min, and solvent volume of 100


Author(s):  
G. A. Zakabluk ◽  
V. V. Koval ◽  
A. A. Chernonosov

Aims: Edoxaban is a direct-acting oral anticoagulant, being a highly selective, direct and reversible factor Xa inhibitor. Edoxaban is used to treat and prevent blood clots such as deep vein thrombosis and pulmonary embolism. The dried spot technic, including dried blood spots and dried plasma spots, is used in many fields, from newborn screening to monitoring of therapeutic drugs in toxicology. In this case, equipment with a highly sensitive detector, such as a mass spectrometer, is required, as well as conditions for a high degree of drug recovery from the dried spot. In this work, the extraction of edoxaban from dried plasma spots (DPS) was studied to determine the optimal parameters of the extraction method. Study Design: Analytical experimental study. Short Research Articles. Place and Duration of Study: Core Facility of Mass Spectrometric Analysis, Institute of Chemical Biology and Fundamental Medicine SB RAS, between August and October 2020 Methodology: The organic extraction method was selected for evaluation as the most suitable for LC-MS analysis. Several parameters were investigated to find the best combination for extracting edoxaban from DPS for further LC-MS analysis: percent organic solvent, presence or absence of 0.1% formic acid (FA), extraction time, volume, and temperature. Results: The results showed that the extraction was influenced by the composition and volume of the solvent, but not temperature and time. Pure acetonitrile is the worst solvent for extracting edoxaban from DPS. The most optimal parameters are MeOH: 0.1% FA in H2O (70:30, v:v) solvent with an extraction temperature of 40 °C, an extraction time of 15 minutes and a solvent volume of 50 μl. Conclusion: Several solvents suitable for LC-MS analysis can be used to recover edoxaban from DPS.


2015 ◽  
Vol 2015 ◽  
pp. 1-10 ◽  
Author(s):  
Lanqing Li ◽  
Mingxing Sun ◽  
Hui Zhou ◽  
Yun Zhou ◽  
Ping Chen ◽  
...  

A rapid and cleanup-free ultrasound-assisted extraction method is proposed for the simultaneous extraction of oxytetracycline, tetracycline, chlortetracycline, and doxycycline in manure. The analytes were determined using high-performance liquid chromatography with ultraviolet detector. The influence of several variables on the efficiency of the extraction procedure was investigated by single-factor experiments. The temperature, pH, and amount of extraction solution were selected for optimization experiment using response surface methodology. The calibration curves showed good linearity (R2>0.99) for all analytes in the range of 0.1–20 μg/mL. The four antibiotics were successfully extracted from manure with recoveries ranging from 81.89 to 92.42% and good reproducibility (RSD, <4.06%) under optimal conditions, which include 50 mL of McIlvaine buffer extraction solution (pH 7.15) mixed with 1 g of manure sample, extraction temperature of 40°C, extraction time of 10 min, and three extraction cycles. Method quantification limits of 1.75–2.32 mg/kg were obtained for the studied compounds. The proposed procedure demonstrated clear reductions in extraction time and elimination of cleanup steps. Finally, the applicability to tetracyclines antibiotics determination in real samples was evaluated through the successful determination of four target analytes in swine, cow manure, and mixture of animal manure with inorganic fertilizer.


2019 ◽  
Vol 78 ◽  
pp. 02011
Author(s):  
Songling Cai ◽  
Min Pang

This paper investigated the effects of liquid-solid ratio, extraction time, extraction temperature and alkali concentration on the extraction rate of millet bran polysaccharides by the enzymatic hydrolysis and alkaline extraction method, then the L9 (34) orthogonal test was designed to optimize the extraction process according to the single factor experiment.The optimum parameters were obtained as follow: 15:1 liquid-solid ratio, five hours extraction time, 80° extraction temperature, and 0.7 mol/l concentration of sodium hydroxide. The extraction rate of millet bran polysaccharide reached 11.46% through the verification experiments under these conditions,and the RSD was 1.79%. Therefore, it can provide some experimental basis for the scientific research of millet bran polysaccharides in the future.


Author(s):  
Nithyakalyani K

Ficus benghalensis is one of those taboo plants in India, which was claimed to be possessed and have weird effects on human health. Apart from this ficus species has a great variety of chemical constituents and an abundant amount of antioxidants. Drying is the most critical stage of improving the activity or preventing the loss of chemical components from a drug. There is another stage of ensuring high chemical constituent content in the plant and that is the extraction procedure. So the point of focus in the current research is to find the effect of extraction method and drying on the anti-inflammatory potential of the plant. The result of the extraction method and drying method of the plant was investigated and found that the ultrasound-assisted extraction of the shade dried leaves was found to give the highest yield of flavonoids and activity.


2021 ◽  
Vol 19 (1) ◽  
pp. 653-664
Author(s):  
Grażyna Kowalska ◽  
Radosław Kowalski

Abstract The objective of this study was the estimation of the content of 13 mycotoxins (diacetoxyscirpenol, T-2 toxin, HT-2 toxin, nivalenol, deoxynivalenol, 3-acetyldeoxynivalenol, fusarenone X, aflatoxin B1, aflatoxin B2, aflatoxin G1, aflatoxin G2, ochratoxin A, and zearalenone) in various products from the eastern part of Poland. The content of mycotoxins in the analysed samples was assayed using the extraction method combined with HPLC-MS/MS analysis. We found mycotoxins in 25 of the 92 samples tested (27%). Contamination with mycotoxins was noted most frequently in samples of cereals – 56% – and also in samples of flour and cocoa, in which a content of mycotoxins was noted in 24 and 16% of the samples, respectively. The most frequently identified were the following – deoxynivalenol detected in 18 samples (72%), zearalenone detected in eight samples (32%), toxin HT-2 detected in four samples (16%), ochratoxin A identified in three samples (12%), and toxin T-2 detected in one sample (4%). In one analysed sample of mixed flour and in one analysed sample of wheat and rye flour, the maximum allowable concentration was exceeded in the case of two identified mycotoxins – deoxynivalenol (2,250 μg/kg) and ochratoxin A (15.6 and 17.1 μg/kg).


Separations ◽  
2021 ◽  
Vol 8 (4) ◽  
pp. 53
Author(s):  
Clarissa Braccia ◽  
Bhakti Prinsi ◽  
Mara Colzani ◽  
Alessandra A. Altomare ◽  
Luca Espen ◽  
...  

The benefits of ginseng have been mainly attributed to its triterpenoids, called ginsenosides. Recent genome sequencing of the Panax ginseng has paved the way for in-depth proteomic studies of this medicinal plant. The current study was conducted to deepen the proteomic information on the root proteome of Korean ginseng. Proteomic workflow was optimized by testing two different strategies, characterized by the phenol extraction procedure, the presence or the absence of SDS-PAGE fractionation step, and nano-scale liquid chromatographic tandem mass spectrometry (nLC-MS/MS) analysis. The results highlighted an evident improvement of proteome extraction by the combination of phenol extraction with SDS-PAGE before the nLC-MS/MS analysis. In addition, a dramatic impact of the steaming process (the treatment to produce red ginseng from ginseng) on protein properties was observed. Overall, the analyses of Korean ginseng permitted the characterization of a total of 2412 proteins. A large number of identified proteins belonged to the functional categories of protein and carbon/energy metabolism (22.4% and 14.6%, respectively). The primary and secondary metabolisms are major metabolic pathways, which emerged from the proteomic analysis. In addition, a large number of proteins known to play an important role in response to (a)biotic stresses were also identified. The current proteomic study not only confirmed the previous transcriptomic and proteomic reports but also extended proteomic information, including the main metabolic pathways involved in Korean ginseng.


2011 ◽  
Vol 704-705 ◽  
pp. 302-307
Author(s):  
Lei Xu ◽  
Guang Ze Dai ◽  
Xing Ming Huang ◽  
Jing Han ◽  
Jun Wen Zhao

Numerical simulation of connecting rod die forging processing was performed by finite element method (FEM) software Deform 3D. The changes of the temperature fields, stress fields of the billet and dies, and upper setting force-stroke curve during the die forging were obtained. The simulation results show that (1) the increase of the fillet radius of dies could effectively reduce the stress concentration so that to prevent the die crack arising at high level stress; (2) the optimum parameters of die forging process are 430°C for forging temperature, 200°C for preheat temperature of dies and 80mm/s for reduction rate by comparing both fields of the stress and temperature during different forging process..


Molecules ◽  
2021 ◽  
Vol 26 (9) ◽  
pp. 2494
Author(s):  
Wei Wang ◽  
Yu-Ting Gao ◽  
Ji-Wen Wei ◽  
Yin-Feng Chen ◽  
Qing-Lei Liu ◽  
...  

In this paper, ultrasonic cellulase extraction (UCE) was applied to extract polyphenols from passion fruit. The extraction conditions for total phenol content (TPC) and antioxidant activity were optimized using response surface methodology (RSM) coupled with a Box-Behnken design (BBD). The results showed that the liquid-to-solid ratio (X2) was the most significant single factor and had a positive effect on all responses. The ANOVA analysis indicated quadratic models fitted well as TPC with R2 = 0.903, DPPH scavenging activity with R2 = 0.979, and ABTS scavenging activity with R2 = 0.981. The optimal extraction parameters of passion fruit were as follows: pH value of 5 at 30 °C for extraction temperature, 50:1 (w/v) liquid-to-solid ratio with extraction time for 47 min, the experimental values were found matched with those predicted. Infrared spectroscopy suggested that the extract contained the structure of polyphenols. Furthermore, three main polyphenols were identified and quantified by HPLC. The results showed the content of phenolic compounds and antioxidant activity of the optimized UCE were 1.5~2 times higher than that determined by the single extraction method and the Soxhlet extraction method, which indicates UCE is a competitive and effective extraction technique for natural passion fruit polyphenols.


Sign in / Sign up

Export Citation Format

Share Document