Phenanthrene-Enriched Extract from Eulophia Macrobulbon Using Subcritical Dimethyl Ether for Phosphodiesterase-5A1 Inhibition

Eulophia macrobulbon (E.C.Parish & Rchb.f.) Hook.f. contains a natural PDE5A1 inhibitor, the phenanthrene, 1-(4'-hydroxybenzyl)-4,8- dimethoxyphenanthrene-2,7-diol (HDP) a potential treatment for erectile dysfunction. This investigation aimed to improve extraction efficiency of HDP from E. macrobulbon by using greener extraction methodology, subcritical fluid dimethyl ether extraction (sDME) rather than classical solvent extraction (CSE) and ultrasound-assisted extraction (UAE). The efficiency and quality of obtained extracts were evaluated by: %process yield; solvent amount; extraction period; temperature; %HDP content by LC-MS assay, bioactivity as inhibition of phosphodiesterase-5A1 (PDE5A1) by radio-enzymatic assay; and chemical profiles by LC-QTOF-MS analysis. sDME yielded the highest content of HDP in the extract at 4.47%, much higher than using ethanol (0.4-0.5%), ethyl acetate (1.2-1.7%), or dichloromethane (0.7-1.4%). Process yield for sDME (1.5-2.7%) was similar or less than that observed with other solvents (0.9-17%), but providing that process yield is not prohibitively low, concentration is a more important metric for clinical application. Optimal sDME extraction conditions were: extraction period, 40 mins; 200% water as a cosolvent; sample-to-solvent ratio of 1:8; temperature, 35°C. Phenanthrene aglycone and glycoside derivatives were major constituents in sDME extracts and lesser amounts of phenolic compounds and sugars. Inhibition of PDE5A1 by sDME (IC50 0.67±0.22 µg/mL) was 10-fold more potent than the ethanolic extract and other extraction methods, suggesting a high likelihood of clinical efficacy. Thus, sDME was more efficient, faster, solvent-sparing, greener extraction methodology and more selective for phenanthrene when extracted from E. macrobulbon.

Active pyridinium based ionic liquid anchored quinuclidine organocatalyst for Morita-Baylis-Hillman reaction

: In the present manuscript, we easily synthesized three different types of ionic liquid supported 3-quinuclidinone organocatalysts such as [PyAmEQ][BF4] (Py-CATALYST-1), [PyAmEQ][PF6] (Py-CATALYST-2), and [PyAmEQ][NTf2] (Py-CATALYST-3). After performing the careful characterization of the above catalysts with sophisticated analytical techniques, we utilized them as a catalyst to study the passive Morita-Baylis-Hillman reaction. The corresponding Morita-Baylis-Hillman adducts were easily isolated, followed by the simple ether extraction method. Moreover, the above protocol also promoted low catalyst loading, short reaction time, wide substrate scope, easy product, and catalyst recycling. We easily recycled the catalytic system for 5 runs with no noticeable loss in the chemical yield. Additionally, Py-CATALYST-3 was also used to prepare biologically active materials, i.e., N-((E,3S,4R)-5-benzylidene-tetrahydro-4-hydroxy-6-oxo-2H-pyran-3-yl) palmitamide derivatives.

Enhancement of Lipid Extraction from Soya Bean by Addition of Dimethyl Ether as Entrainer into Supercritical Carbon Dioxide

Soya beans contain a variety of lipids, and it is important to selectively separate neutral lipids from other lipids. Supercritical carbon dioxide extraction has been used as an alternative to the selective separation of neutral lipids from soya beans, usually using non-polar hexane. However, supercritical carbon dioxide extraction has a high operating pressure of over 40 MPa. On the other hand, liquefied dimethyl ether extraction, which has attracted attention in recent years, requires an operating pressure of only 0.5 MPa, but there is concern about the possibility of an explosion during operation because it is a flammable liquefied gas. Therefore, this study aims to reduce the operating pressure by using a non-flammable solvent, supercritical carbon dioxide extraction mixed with liquefied dimethyl ether as an entrainer. The extraction rate and the amount of neutral lipids extracted increased with increasing amounts of added liquefied dimethyl ether. In the mixed solvent, the amount of neutral lipids extracted was higher at an operating pressure of 20 MPa than in pure supercritical carbon dioxide extraction at 40 MPa. The mixing of liquefied dimethyl ether with supercritical carbon dioxide allowed an improvement in the extraction of neutral lipids while remaining non-flammable.

Single-Laboratory Validation Study of a Rapid TD-NMR method for Quantitation of Total Fat in Sunflower Oil Powder

Background A rapid total fat quantitation method for sunflower oil powder was developed using time domain nuclear magnetic resonance (TD-NMR). Currently, industry has three major methods for the total fat quantitation: gravimetric analysis after ether extraction (AOAC 933.05 and 989.05), gas chromatography with flame ionization detector (GC-FID AOAC 996.06), and high resolution NMR. The gravimetric analysis method takes a day using highly flammable solvents, and the GC-FID method takes two days requiring harsh chemicals for hydrolyzation, extraction, and methylation. High resolution NMR spectroscopy method requires simpler sample preparation and shorter analysis time compared to the other two methods. Often, only required sample preparation step is to dissolve a sample in a solvent. The acquisition time depends on types of analyzing nuclei and sample. The vegetable oil analysis by 13C NMR takes about four hours per sample. 1H NMR usually takes less time to analyze. In contrast, TD-NMR relaxometry method takes only an hour to prepare and analyze samples if the test is for total fat only. The acquisition time is 40 s per sample, and samples are analyzed “as is”. A rapid analysis method in a quality control laboratory is very crucial for laboratory efficiency in releasing products. In this paper, a single-laboratory validation study is described for a rapid TD-NMR method to quantitate total fat in sunflower oil powder. Objectives This validation work is to provide documented evidence for the method validity as well as the method performance. Methods The method used Bruker minispec mq-20 NMR analyzer® with minispec plus® software. Hahn-echo pulse program was used in the method to collect spin echo signal to determine total fat content. Results The linearity/range result from ten standards (0, 21, 42, 63, 83, 92, 100, 108, 117, and 125%) has the coefficients of determination (R2) of 1.0000. The 100% level is 1.2 g of fat in 2.5 g sample, which is targeted fat content in a sunflower oil powder raw material. The method is specific for the quantitation of total fat in sunflower oil powder with no background interference from the matrix. The precision result of the six replicate samples at 100% level is 0.3% RSD. The accuracies measured from triplicate analysis of 80, 100, and 120% sample matrices are 100, 100, and 100% average recoveries, respectively. The ruggedness of the test method is 0.4% RSD of 12 analysis from two analysts (6 results from each analyst) on the different days. Conclusions The test method is proven to be specific, linear, precise, accurate, rugged, and suitable for intended use of quantitative analysis for total fat in sunflower oil powder. Highlights Traditional methods of gravimetric or GC-FID for total fat analysis of raw materials require lengthy sample preparation and experiment time. Laboratory needs to spend a day to perform gravimetric analysis following ether extraction method and 2 days for GC-FID method. In addition, these test methods use highly flammable and harsh chemicals that generate hazardous chemical wastes. These hazardous wastes are harmful to analysts and environments. In contrast, TD-NMR method is safe, environmentally friendly, and fast. Therefore, TD-NMR is a preferred method for quality control laboratories.

Analytical method development and validation studies for estimation of anti-psychotic drug (Olanzapine)

<p class="abstract"><strong>Background:</strong> Various sophisticated strategies have been raised in conformity with permit the fast separation and quantification about clue aspects concerning complex mixtures of biological matrix. These needs underscored the necessary of analytical instrumentation and the creation of new strategies.</p><p class="abstract"><strong>Methods:</strong> A rapid, accurate, precise, and simple UV then LC-MS/MS analytical methods has been flourished for the determination of Olanzapine (OLZ) in tablet formulation. </p><p class="abstract"><strong>Results:</strong> Chromatographic separation was conducted out on a Phenomenex 250×4.60 mm with an isocratic mobile phase consisting formic acid of 0.1% v/v in Methanol and water at a ratio regarding 92:08v/v and an aggregation run time of 2.5 min. The plasma Olanzapine concentrations were quantified the use of SCIEX API 3000 LC-MS/MS provision geared up along electro spray ionization cleft into the multiple reaction limit mode at m/z 313.4 to 256.3 for Olanzapine; and m/z 327.1 to 270.0 for clozapine respectively. Calibration requirements were organized into the range 5 ng/ml in conformity with 1000 ng/ml for Olanzapine. The effects had been unique and reproducible with the samples prepared by way of liquid-liquid extraction method using Tert-butyl methyl ether extraction in the course of approach improvement trials.</p><p class="AT"><strong>Conclusions:</strong> The novelty on its technique entails the improvement and validation by means of the usage of some quadrant easy pattern decontamination approach and the most sensitive technique with shortest analysis time.</p>

The petroleum ether extraction of Brassica Rapa L. induces apoptosis of Lung adenocarcinoma cells via mitochondria-dependent pathway

Brassica rapa L. is one of the most popular traditional food with a variety of biological activities. In this study, the petroleum ether extract of B. rapa was separated by...

Effect of Oil Content in Tea-seed Pancake on the Determination of Tea Saponin

According to the national standard for the determination of tea saponin content in tea-seed pancake (GB/T 35131-2017), tea saponin was obtained by extracting oil with ethanol and removing solvent. The actual samples of tea-seed pancake did not completely remove the oil, and some of the residual oil content was as high as 9%. Due to the long period of national standard determination, people often use ethanol to extract tea saponin directly, instead of subsequent acid hydrolysis or alkali hydrolysis steps, so as to realize the rapid evaluation of tea-seed pancake quality. In this case, the residual oil has a greater impact on the results. If it was still tested according to the national standard method, the result will be much higher than the actual result. In this work, petroleum ether extraction process was selected before ethanol extraction to remove the residual oil. Experimental results showed that, the accuracy of the determination was effectively improved.