Chloroform-soluble extracts

It is to be noted that the magnitude of the increase in each of the measured properties, between the initial and maximum values, was quite different for the subbituminous coal and the three bituminous coals. Examples of the increases from the initial value (determined for the chloroform-soluble extract from the parent coal) to the maximum are the 0/A ratio increased from 0.8 initial value to 8.0 maximum value for the subbituminous coal, PSOC-1403, and from 0.25 to 1.5 for the bituminous coal, PSOC-1266 the H/C atomic ratio increased from 1.46 to 1.60 for the subbituminous coal, PSOC-1403, and from 1.01 to 1.06 for the bituminous coal, PSOC-1266 (see Figure 2). 

Analyses of the chloroform-soluble extracts of the subbituminous coal by Fourier transform infrared spectroscopy (FTIR) showed the presence of a sharp carbonyl absorption peak (1800-1650 cm ) in the extracts from the parent coal and in those obtained at yields less than about 10% wt dmmf. The peak, which is attributed to ketones and carboxylates, disappeared at higher conversions (16). Whitehurst and co-workers (12) established that carbonyl- containing compounds, such as esters and carboxylates, can cleave under thermal treatment to produce CO, CO2 and phenols. They concluded that the evolution of these gases during coal liquefaction could originate from the decomposition of similar oxygen functionalities in the coal. 

Activity-monitored fractionation of a chloroform-soluble extract of Deprea subtriflora using a quinone reductase induction assay led to the C-18 norwithanolides mentioned previously. Six of the active compounds obtained from this plant (44, 46, 47, 49, 52 and 53), presentes an a,P-unsaturated ketone unit in ring A. Compound 55 -with a doubly unsaturated ring A ketone- was found to be inactive in the QR assay, while compound 54 was active [72]. It has been suggested that the presence of an a,p-unsaturated ketone unit in ring A of withanolides is important for inducing activity in the cell-based QR induction assay,... 

Following the same procedures described in the above-mentioned study, additional extractive data were obtained for the epoxy phenolic enamel that was irradiated at 4.7-7.1 Mrad at 25 and — 30 °C in the presence of distilled water, 3% acetic acid, and n-heptane. The changes in the amount of extractives resulting from the irradiation treatment are shown in Table IX. In the case of the water and acetic acid extractives, there was no change in either the chloroform-soluble fractions or the chloroform-insoluble fractions. In the case of the n-heptane extractives, the amount of extractives decreased when the irradiation temperature was reduced from +25 to — 30°C. Infrared spectra of the chloroform-soluble residues from the water and acetic acid extractives of the unirradiated and irradiated enamel were identical to the chloroform-soluble residues from the solvent blanks. In other words, the epoxy phenolic... 

The active chloroform-soluble residue (6.2 g) was separated into tertiary phenolic and nonphenolic fractions by dissolving the residue in 250 ml of chloroform and extracting three times each with 250 ml of 5% sodium hydroxide solution. After drying, the chloroform solution was evaporated to leave 4.7 g of tertiary nonphenolic alkaloids that possessed all of the antimicrobial activity. 

Along with epi-eudesmanes, 25-27, alloaromadendranes 58-60 were separated from the chloroform solubles of a methanol extract of A. cannabina [36], As was the case with axisonitrile-2 (53), extensive spectroscopic analyses including Eu(fod)3 shift reagent experiments in XH- and 13C NMR permitted assignment of relative stereochemistry. Acanthella pulcherrima was also a source of isothiocyanate 59, although both isonitrile and formamido compounds appear to be absent [20],... 

Preliquefaction at 275 C appears to have a negative effect on subsequent liquefaction when compared to results without a preliquefaction step. Preliquefaction results in up to 10% of the coal converted to gases and chloroform solubles. Most coals behaved the same and there was little effect due to the presence of either the catalyst or hydrogen. The solvent was, however, necessary to produce the chloroform extracts as none were produced by a thermal treatment in the absence of a solvent. 

C]PCNB metabolism was studied in vivo with 30-day-old peanut plants grown in nutrient solution that contained 17.6 ppm [I CjPCNB. Plant tissue was extracted with cold 80t methanol 48 hr after final exposure to PCNB. The extracts were made aqueous and partitioned against chloroform at pH 5.5 and against ethyl ether at pH 2. Water-soluble, chloroform-soluble, and ether-soluble metabolites were isolated by various chromatographic methods and identified by mass spectrometry and/or by synthesis. The details of these studies have been published previously (, X ... 

Catalase inhibition. Water extract of the fresh root, administered intragastrically to infant mice at a dose of 50 mL/kg, was active. The treatment was administered for seven successive days, followed by a single dose of 20% v/v CCI4 in olive oil subcutaneously at 1 mL/kg on the last day 1 hour after the administration of the carrot extract " . Chloroform-methanol (9 1) fraction of the ethanol (95%) extract, ethyl acetate fraction of the water extract, and chloroform-soluble fraction of the water extract of the seed were active on the nonpregnant rat uterus° L... 

Samples of both the bromide and chloride crude reaction mixtures were extracted with anhydrous chloroform to obtain a chloroform-soluble residue. Chloroform extraction was chosen here, because the niobium (IV) adducts appeared to be substantially insoluble in this solvent. Samples of the soluble residue were dissolved in anhydrous chloroform for infrared analysis. The resulting absorption spectra were then compared to those obtained in the same way for known samples of pyridinium chloride and bromide (Table VI). 

Table 4. Effects of varions lipid fractions of chloroform methanol extract (1 1,v/t) (a), acetone- soluble and -insoluble fractions (b), and n-hexane-soluble and -insoluble fractions (c) on tumor volume at 20 d and tumor weight at 21 din sarcoma 180-bearing mice1...

The other experiment was performed by Isaksson (5) earlier. He extracted desiccated bile, using different solvents in succession. With chloroform, all of the lecithin was extracted but was accompanied by a large part of the bile salts. While bile salts by themselves are insoluble in chloroform, the extract thus obtained contains a proportion by weight of 2 parts of bile salt to 1 of lecithin—about one molecule of lecithin for three molecules of bile salt. Here, it is the lecithin, soluble in chloroform because of its paraffinic chains, which by association solubilizes the bile salt. It is interesting to inquire how these associations are achieved in both cases—i.e., how the molecules of bile salt are arranged and oriented in relation to the molecules of lecithin and to the polar or non-polar solvent. Let us examine first the state of the bile salt molecules in an aqueous phase. 

The infrared spectra of the coal and the various extracts were recorded on a Baird, Model GY-1 (Ireland Mine vitrain concentrate) and on a Perkin Elmer Model 337 spectrophotometer (Bruceton coal). The samples were prepared by the potassium bromide pellet technique. The high resolution proton NMR spectrum of the benzene soluble extract from Ireland Mine vitrain concentrate was recorded on a Varian A-60 spectrometer in 10% deuterated chloroform (CDCh) solution, using tetrametnylsilane internal standard. 

The solubility of NHDC in hot water, alcohol, aqueous alkali, acetonitrile, dimethyl sulfoxide, and alcohol/water mixture facilitates its selective extraction from food samples (20,91,94). It is extracted from jams, fruit juices, and dairy products with methanol (66,93) or acetone (95) and filtered or centrifuged. Chewing gum samples are dissolved in chloroform and extracted with water. The extract is centrifuged, and the clear supernatant is injected into the HPLC (95). If necessary, sample cleanup and concentration may be achieved by selective adsorption or desorption (20) on Sep-Pak Cl8 (96). Tomas-Barberan et al. (93) used Amberlite XAD-2 resin for purification of jam extract. Sugars, pectin, and other polar compounds were eluted with water, and NHDC was eluted with methanol. After concentration, the extract was further purified on a Sephadex LH-20 column prior to HPLC analysis. 

Table IX shows the solublity of the herbicides in various solvents. If the extraction process is based on a solvation mechanism then a non-polar solvent (such as chloroform) should extract these solutes better than a more polar solvent (such as methanol or water).

Lund and DeLuca (101) administered [ H] vitamin D3 to rats and found biologically active metabolites in the bone, liver and serum. The aqueous-soluble metabolites from the tissues and the feces did not have vitamin D activity. At least three biologically active metabolites were isolated from the chloroform-soluble portion of the extract. One of these was found in large amounts in the liver, blood and bone. In 1968, Blunt et. al. (102) proved convincingly that this major metabolite is 25-hydroxyvitamin D3 (25-OH-D3). Two other groups of investigators (103,104) independently found clues to the metabolic hydroxylation of vitamin Do. It was soon established that 25-hydroxylation of vitamin D3 takes place primarily in the liver (105,106) and that 25-0H-D3 is the major form of circulating vitamin D3 in human plasma (107). 

A solution of betamethasone (1.0 g) in dry tetrahydrofuran (40 ml) was treated with adamantane carbonyl chloride (about 2.2 equivalents) in dry tetrahydrofuran (5 ml) and then pyridine (0.8 ml) was added. The mixture was refluxed for 6 h and then most of the solvent was boiled off and the residue extracted with chloroform to afford a froth. The ether soluble portion of this froth was dissolved in chloroform and extracted repeatedly with dilute sodium bicarbonate solution. Evaporation of the chloroform layer gave a froth which was further purified by chromatography and crystallisation from chloroform-petroleum ether to yield betamethasone 21-adamantane-l -carboxylate melting point 256°-259°C (dec.). 

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