scholarly journals Optimization of the Extraction Procedure of Apixaban from Dried Rat Plasma Spots

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):  
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):  
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.


2014 ◽  
Vol 58 (11) ◽  
pp. 6747-6757 ◽  
Author(s):  
Teresa L. Parsons ◽  
Mark A. Marzinke ◽  
Thuy Hoang ◽  
Erin Bliven-Sizemore ◽  
Marc Weiner ◽  
...  

ABSTRACTThe quantification of antituberculosis drug concentrations in multinational trials currently requires the collection of modest blood volumes, centrifugation, aliquoting of plasma, freezing, and keeping samples frozen during shipping. We prospectively enrolled healthy individuals into the Tuberculosis Trials Consortium Study 29B, a phase I dose escalation study of rifapentine, a rifamycin under evaluation in tuberculosis treatment trials. We developed a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for quantifying rifapentine in whole blood on dried blood spots (DBS) to facilitate pharmacokinetic/pharmacodynamic analyses in clinical trials. Paired plasma and whole-blood samples were collected by venipuncture, and whole blood was spotted on Whatman protein saver 903 cards. The methods were optimized for plasma and then validated for DBS. The analytical measuring range for quantification of rifapentine and its metabolite was 50 to 80,000 ng/ml in whole-blood DBS. The analyte was stable on the cards for 11 weeks with a desiccant at room temperature and protected from light. The method concordance for paired plasma and whole-blood DBS samples was determined after correcting for participant hematocrit or population-based estimates of bias from Bland-Altman plots. The application of either correction factor resulted in acceptable correlation between plasma and whole-blood DBS (Passing-Bablok regression corrected for hematocrit;y= 0.98x+ 356). Concentrations of rifapentine may be determined from whole-blood DBS collected via venipuncture after normalization in order to account for the dilutional effects of red blood cells. Additional studies are focused on the application of this methodology to capillary blood collected by finger stick. The simplicity of processing, storage, shipping, and low blood volume makes whole-blood DBS attractive for rifapentine pharmacokinetic evaluations, especially in international and pediatric trials.


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.


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.


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.


2014 ◽  
Vol 955-959 ◽  
pp. 3377-3380 ◽  
Author(s):  
Qing Chen ◽  
Te Wang ◽  
Jin Dan Zhao ◽  
Fu Hui Kang ◽  
Yi Ming Zhang ◽  
...  

The simultaneously co-production of Poly-β-hydroxybutyrate (PHB) and ectoine in a process (PHB/Ect co-production) and co-products extraction have great significant for reducing the manufacture cost and promoting industrialization of PHB and ectoine. The pure aqueous extraction method based on osmotic downshock was used for the extraction of PHB/Ect co-products byH. salina. The effects of osmotic pressure, extraction temperature and extraction time on the extraction rate of PHB were investigated. The ectoine was extracted and purified by the techniques of hollow fiber and ion exchange. The optimal conditions for PHB extraction were osmotic downshock in pure water, extraction temperature at 60 °C and extraction for 4 h. The extraction rate of PHB was 87.5%. The extraction rate of ectoine was 84.2%.


2013 ◽  
Vol 295-298 ◽  
pp. 150-154
Author(s):  
Feng Jie Wang ◽  
Xin Qiao Dong ◽  
Xiao Liu

Development natural pigment retained a variety of nutrition composition is extremely research value.Water Wax Trees Fruit was as raw materials,citric acid aqueous solution was as extracting agent.Amaranthine pigment extraction method were studied on fully grasping the stability of the natural amaranthine pigment and no damage to the water wax fruit biological activity.The effect of extraction yield were studied on Water Wax Trees Fruit natural amaranthine pigment.The results show that the better extraction conditions are extraction temperature at 70 °C, extraction time for 3h,citric acid concentration1.0 % , the material/liquid ration(g/ml) 1:5.The extraction yield is 2.95%.Ultraviolet absorption maximum wavelength is 280 nm.


2018 ◽  
pp. 75-82 ◽  
Author(s):  
Мухендис (Mukhendis) Мамедгусейин оглы (Mamedgusejin ogly) Джахангиров (Cahangirov) ◽  
Микаил (Mikail) Акпер оглы (Аkper ogly) Магеррамов (Маharrаmov)

It was shown that the scent and taste of tea are determined by the level of protein and amino acid. Certainly, protoingens that make up most part of proteins are noted among amino acids. All of them are considered L-shaped. Green tea mostly consists of proteins. Even the high level protein doesn’t adversely impact the quality of tea yet that of black tea might be negatively influenced by that. Also, its taste will also be worsened by that.As a result of analysis 16 amino acids and 8 unsubstituted substance was found. The main part of amino acid is taken by teanin. It take 41.3% of Azerbaijan-1, 38.8% of Kolxida types respectively. In all stages of tea leaf processing the decrease of teanin and increase of glutamin is witnessed. Also, the loss of teanin happens during the purification (by 34%) and the fading stages.As a result of the work carried out, it has been found that the size of the tea leaf particle, the temperature and the extraction time influence the extraction of the theanine. The optimum are: the size of the tea leaf particle is 200–450 mkm, the extraction temperature is 80–85 °C, and the extraction time is 20–25 minutes.


2001 ◽  
Vol 84 (2) ◽  
pp. 309-316 ◽  
Author(s):  
Nadiá M Jones ◽  
M Gabriela Bernardo-Gil ◽  
M Graço Lourenco

Abstract Ultrasound and microwave techniques were used to extract tobacco alkaloids, and response surface methodology was used to optimize extraction conditions. Ultrasonic technique factors were temperature, 30–85°C; time, 3–45 min; solvent volume, 8–80 mL. Microwave extraction factors were pressure, 15–75 psi; time, 3–40 min; power, 30–90% of the maximum magnetron power of 650 W. Soxhlet and solvent AOAC-modified extraction methods were also applied after some improvements. Nicotine, nornicotine, anabasine, and anatabine were quantified by gas chromatography. A steam distillation International Standards Organization method for total alkaloid evaluation was used as reference. The results obtained by the different methods were compared using a least squares deviation test. The ultrasonic and the proposed modified-AOAC extraction method were the more convenient with regard to practicability and precision. The relative deviations (n = 5) were as follows: For the ultrasonic method in low-level alkaloid tobaccos, 0.7% nicotine and 1.4–14% minor alkaloids; in high-level alkaloid tobaccos, 2.4% nicotine and 4.5–5.1% minor alkaloids. For the modified AOAC method in low-level alkaloid tobaccos, 0.9% nicotine and 2.4–11.6% minor alkaloids; and in high-level alkaloid tobaccos, 1.7% nicotine and 2.0–2.4% minor alkaloids.


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