Ethyl acetate identification

The above example serves to iUustrate the basis of the procedure employed for the characterisation of aUphatic esters, viz., hydrolysis to, and identification of, the parent acids and alcohols. Most esters are liquids a notable exception is dimethyl oxalate, m.p. 54°. Many have pleasant, often fruit-hke, odours. Many dry esters react with sodium, but less readily than do alcohols hydrogen is evolved particularly on warming, and a sohd sodio derivative may separate on coohng (e.j/., ethyl acetate yields ethyl sodioacetoacetate ethyl adipate gives ethyl sodio cj/cZopentanone carboxylate). 

Norethindrone may be recrystakhed from ethyl acetate (111). It is soluble in acetone, chloroform, dioxane, ethanol, and pyridine slightly soluble in ether, and insoluble in water (112,113). Its crystal stmcture has been reported (114), and extensive analytical and spectral data have been compiled (115). Norethindrone acetate can be recrystakhed from methylene chloride/hexane (111). It is soluble in acetone, chloroform, dioxane, ethanol, and ether, and insoluble in water (112). Data for identification have been reported (113). The preparation of norethindrone (28) has been described (see Fig. 5). Norethindrone acetate (80) is prepared by the acylation of norethindrone. Norethindrone esters have been described ie, norethindrone, an appropriate acid, and trifiuoroacetic anhydride have been shown to provide a wide variety of norethindrone esters including the acetate (80) and enanthate (81) (116). 

The identification of bi-layer adsorption of polar solvents on the surface of silica gel arose from some work by Scott and Kucera (5) who measured the adsorption isotherms of the some polar solvents, ethyl acetate, isopropanol and tetrahydrofuran from n-heptane solutions onto silica gel. The authors found that the experimental results for the more polar solvents did not fit the simple mono-layer adsorption equation and, as a consequence, the possibility of bi-layer adsorption on the silica gel surface was examined. 

After the identification of the suitable compound bands, silica gel is scraped off the plates, placed in short glass columns, Pasteur pipettes, or sintered filter funnels, and fractions are recovered with such volatile solvents as ethyl acetate or dichloromethane. 

This procedure was compared with sequential extractive techniques employing alkaline hydrolysis of dried plant tissue followed by extraction of the acidified mixture with ethyl acetate. Fractions were individually evaluated for phytotoxic properties. Selected fractions from those showing a positive response were analyzed by gas-liquid chromatography. Structural identification and characterization of the individual components in these selected fractions were accomplished by gas chromatography-mass spectrometry. 

A new HP-TLC method has been applied for the quantitative analysis of flavonoids in Passiflora coerulea L. The objective of the experiments was the separation and identification of the compound(s) responsible for the anxiolytic effect of the plant. Samples were extracted with 60 per cent ethanol or refluxed three times with aqueous methanol, and the supernatants were employed for HPTLC analysis. Separation was performed on a silica layer prewashed with methanol and pretreated with 0.1 M K2HP04, the optimal mobile phase composition being ethyl acetate-formic acid-water (9 1 l,v/v). It was established that the best extraction efficacy can be achieved with 60 - 80 per cent aqueous methanol. The HPTLC technique separates 10 different flavonoids, which can be used for the authenticity test of this medicinal plant [121],... 

A simple TLC method has been developed for the separation and identification of flavons and flavon glycosides in the extract of Phillyrea latifolia L. The leaves (100 g) were defatted in 11 of chloroform for 24 h and then extracted with 2 X 11 of ethanol-water (80 20, v/v). The collected extracts were concentrated and extracted again with n-hexane to remove chlorophylls and other apolar constituents. Analytes were extracted with ethyl acetate. Both normal phase and RP-TLC have been used for the separation of flavonoids. The results are compiled in Table 2.36. It was concluded from the data that TLC can be successfully applied for the quality control of plant extracts containing various flavone derivatives [124],... 

The separation and identification of two novel anthocyanins from red onion, Allium cepa, have also been reported. Scales of 2.37 kg red onion were cut and extracted twice with methanol containing 0.5 per cent TFA. The extract was filtered, extracted with ethyl acetate and the aqueous phase was further purified in an ion-exchange and an SEC column. SEC separation was performed in a Sephadex LH-20 column (100 X 5 cm i.d.) applying methanol-water-TFA (39.6 60 0.4, v/v) as the mobile phase at a flow rate of 2.5 ml/min. 

Mechanisms for both reactions are proposed, which are supported by the identification of several intermediate reactions. The role of various organic and inorganic reaction promoters is discussed. Amongst these, phosphine oxides are exceptionally efficient in that they induce high reaction rates combined with high selectivities. Reactions a) and b) potentially allow two-step, methanol/ /synthesis gas-based routes to ethyl acetate and proprio-nic acid, respectively. 

The unstable thiazolinones are converted into stable hydantoines in order to facilitate their identification. Conversion and identification are carried out outside the instrument after extraction of the thiazolinones with butylchlor-ide. The conversion reaction as well as the problems associated with identification of the PTH-amino acids were studied in detail by Edman and described explicitly in Needleman s book on Protein Sequence Determination Conversion is generally carried out in 1 N HCl at 80 °C within 10 min. The PTH-derivatives are extracted from the aqueous phase with ethyl acetate with the exception of PTH-arginine, PTH-histidine and PTH-cysteine which remain in the aqueous phase. 

In view of its rapidity we found thin layer chromatography convenient for identification of the amino acids liberated by the first 20—30 degradation cycles. For identification of PTH-derivatives from additional degradation steps we prefer gas-liquid chromatography because of its merits mentioned above, particularly its greater sensitivity. Several colorimetric reactions and chromatographic systems are available for the identification of those PTH-amino acids which remain in the aqueous phase when the PTH-derivatives are extracted with ethyl acetate 23.24,25,13) our hands, thin layer electrophoresis was found to be satisfactory 26,27)... 

Volatile constituents of cupuacu were isolated by steam distillation-extraction of pulp or juice [2].The identification of volatile constituents was based on mass spectral analysis. The pleasant aroma compounds were mainly esters (Fig. 8.2). Targe amounts of ethyl butanoate and small amounts of ethyl acetate, butyl acetate, and butyl isobutanoate were described. 

Three standardized methods were found in the Official Methods ofAnalysis of the Association of Official Analytical Chemists (AOAC 1990). The first of these methods is based on the extraction of crops (kale, endive, carrots, lettuce, apples, potatoes, and strawberries) with ethyl acetate and isolation of the residue followed by a sweep codistillation cleanup prior to GC/thermionic detection (Method 968.24). The second of these methods utilizes Florisil column chromatography clean-up followed by GC/FPD (Method 970.53). In the third method (Method 970.52), the sample is extracted with acetonitrile, and the residue is partitioned into petroleum ether followed by Florisil clean-up and GC/KC1 thermionic detection. Identifications are based on combinations of gas, thin-layer, and paper chromatography. The recovery for diazinon in this method is stated to be greater than 80% no data on limits of detection were given. 

Note Ethyl acetate is a solvent impurity of ether. 900 mL of solvent/700 mL of resin was successively Soxhlet extracted for 24 h with CH3OH, CH3C=N, and ether. No compounds were identified in the ether fractions. A sample was injected directly into the GC-MS. Identifications are tentative no retention time data have yet been correlated. Identifications were completed by MS only. 

The paper-chromatographic properties of the common deoxy and dideoxy sugars have been treated in several reviews,2 28 a book,829 and individual publications. Common solvent-systems are 6 4 3 1-butanol-pyridine-water (Solvent A) 4 1 5 1-butanol-acetic acid-water (Solvent B) and 1-buta-nol-ethanol-water (4 1 5, upper phase, Solvent C or 3 1 1, Solvent D). The four 2-deoxy-D-hexoses and the 2,6-dideoxyhexoses may be separated as their borate complexes. 0 The use of 1-butanol-water on the one hand, and of 2-butanone-borate buffer on the other, usually provides adequate separation and, by use of a combination of solvents, these deoxy sugars may be identified. 80 The use of buffered systems has proved highly advantageous in the separation and identification of the isomeric 6-deoxy-hexoses.8 1 Other systems, such as Solvent A and 2 1 2 ethyl acetate-... 

Another LC-APCI-MS method has been developed and validated by Zhang et al. for the identification and quantification of zaleplon in human plasma using estazolam as an IS. After the addition of estazolam and 2.0 M sodium hydroxide solution, plasma samples were extracted with ethyl acetate and then the organic layer was evaporated to dryness. The reconstituted solution of the residue was injected onto a prepacked Shim-pack VP-ODS C18 (250 mm x 2.0 mm i.d.) column and chromatographed with a mobile phase comprised methanol-water (70 30) at a flowrate of 0.2 ml/min. 

Capsules TLC Shake contents with Silica Ethyl acetate- 254 nm USP 23. identification [5]... 

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