Methanol, derivative detection

The radioactive signals of radio-GC show the 1 -methanol derivates and its common derivates with non radioactive methyl iodide (Fig. lb). The nC-methanol derivates take part in new molecule formation with non-radioactive methyl iodide or/and its derivates on catalyst surface. The C-methyl iodide as a newly formed radioactive product was detected while the selectivity to hydrocarbons sharply decreased (Fig. 2b). 

The reactants and products were separated on an MOS Hypersil column (4.6 millimeters x 200 mm, 5 /urn). The mobile phase was composed of a 90 10 mixture of solvent A, consisting of 0.1 M sodium acetate, 0.02 M citric acid, 0.93 mM sodium octanesulfonate, and 0.12 mM disodium EDTA (pH 4.6), and solvent B, methanol UV detection was used, with the optimal wavelength being 258 nm for the adenoxyl derivatives and 279 nm for adrenaline and noradrenaline. Quantitation was normally based on the S-adenosyl-L-homocysteine formed. 

Reversed-phase hplc has been used to separate PPG into its components using evaporative light scattering and uv detection of their 3,5-dinitroben2oyl derivatives. Acetonitrile—water or methanol—water mixtures effected the separation (175). Polymer glycols in PUR elastomers have been identified (176) by pyrolysis-gc. The pyrolysis was carried out at 600°C and produced a small amount of ethane, CO2, propane, and mostiy propylene, CO, and CH4. The species responsible for a musty odor present in some PUR foam was separated and identified by gc (Supelco SP-2100 capillary column)... 

In some cases, e.g. the detection of antioxidants [6], the plate is heated to 105 °C for 5 min after being sprayed and the still hot plate placed immediately in an ammonia-vapor chamber. The blue color of the tryptamine derivatives is also stabilized by spraying afterwards with a 5% methanolic ammonia solution [12]. 

Note If netilmicin is to be chromatographed alone it is recommended that the methanol content of the mobile phase be increased (e.g. to 23 -I- 7), in order to increase the value of the hRf. The detection limit for the substances in the application tested was more sensitive using DOOB reagent on RP layers than when NBD chloride, fluorescamine or o-phthalaldehyde were employed. The derivatives so formed were stable and still fluoresced after several weeks if they were stored in the dark. 

Note The pre- and post-treatment of the chromatograms with the basic tri-ethylamine solution, which can be replaced by an alcoholic solution of sodium hydroxide [1,4] or a phosphate buffer solution pH = 8.0 (c = 0.2 mol/1) [5], serves to stabilize the fluorescence of the amino derivatives [2]. A final spraying with methanolic hydrochloric acid (chci = 5 mol/1) or 70% perchloric acid renders the detection reaction highly specific for histamine [4] and for catecholamines and indolamines [5]. 

Irradiation of 3-benzoyl-2-methoxy-3//-azepine (32) in methanol gives rise to a mixture of the 3-azabicyclo[4.1.0]hepta-2,4-diene 33 (detected by HNMR spectroscopy, but not isolated), 2-methoxy-3-phenacylpyridine(34), and a trace of 2-phenylfuro[2,3-A]pyridine (35), this last product being an artefact derived from the phenacylpyridine 34.246... 

Detectability may be a significant problem with homologous series of unsaturated compounds, particularly //-alkanes. For these compounds, refractive index detection or evaporative light-scattering, both of which are described elsewhere in the book, may be of use. Indirect photometry is a useful detection scheme for compounds that do not absorb in the UV. Acetone, methylethyl ketone, methyl propyl ketone, methyl isopropyl ketone, methyl isobutyl ketone, and acetophenone are added to an acetonitrile/water mobile phase, generating a negative vacancy peak when the nonchro-mophoric analyte emerges and a positive peak if the ketone is adsorbed and displaced.70 Dodecyl, tetradecyl, cetyl, and stearyl alcohols also have been derivatized with 2-(4-carboxyphenyl)-5,6-dimethylbenzimidazole and the derivatives separated on Zorbax ODS in a mobile phase of methanol and 2-propanol.71... 

Brack [81] has illustrated the analysis of antioxidants in a CB-free vulcanisate of unknown composition according to Scheme 2.7. Some components detected by off-line TD-GC-MS (cyclohexylamine, aniline and benzothiazole) were clearly indicative of the CBS accelerator other TD components were identified as the antioxidants BHT, 6PPD, Vulcanox BKF and the antiozonant Vulkazon AFS. In the methanol extract also the stabiliser ODPA was identified. The presence of an aromatic oil was clearly derived from the GC-MS spectra of the thermal and methanol extracts. The procedure is very similar to that of Scheme 2.3. 

Electrospray mass spectrometry is a technique that allows pre-existing ions to be transferred from solution to the gas phase with minimal fragmentation, followed by conventional mass analysis. Recently electrospray mass spectra have been studied for a number of cationic phos-phinegold(I) complexes in dichloromethane/methanol solution.2525 For derivatives of the types [Au(PR3)2]+ and [Au(PR3)3]+, the intact cations were observed, but ions of the type [Au(PR3)4]+ where not detected in the gas phase. Even the three-coordinated [Au(PR3)3]+ are relatively unstable in the gas phase, and the ions [Au(PR3)2]+ are readily produced. 

Gotti et al. [42] reported an analytical study of penicillamine in pharmaceuticals by capillary zone electrophoresis. Dispersions of the drug (0.4 mg/mL for the determination of (/q-penicillaminc in water containing 0.03% of the internal standard, S -met hy I - r-cystei ne, were injected at 5 kPa for 10 seconds into the capillary (48.5 cm x 50 pm i.d., 40 cm to detector). Electrophoresis was carried out at 15 °C and 30 kV, with a pH 2.5 buffer of 50 mM potassium phosphate and detection at 200 rnn. Calibration graphs were linear for 0.2-0.6 pg/mL (detection limit = 90 pM). For a more sensitive determination of penicillamine, or for the separation of its enantiomers, a derivative was prepared. Solutions (0.5 mL, final concentration 20 pg/mL) in 10 mM phosphate buffer (pH 8) were mixed with 1 mL of methanolic 0.015% 1,1 -[ethylidenebis-(sulfonyl)]bis-benzene and, after 2 min, with 0.5 mL of pH 2.5 phosphate buffer. An internal standard (0.03% tryptophan, 0.15 mL) was added and aliquots were injected. With the same pH 2.5 buffer and detection at 220 nm, calibration graphs were linear for 9.3-37.2 pg/mL, with a detection limit of 2.5 pM. For the determination of small amounts of (L)-penicillamine impurity, the final analyte concentration was 75 pg/mL, the pH 2.5 buffer contained 5 mM beta-cyclodextrin and 30 mM (+)-camphor-10-sulfonic acid, with a voltage of 20 kV, and detection at 220 nm. Calibration graphs were linear for 0.5-2% of the toxic (L)-enantiomer, with a detection limit of 0.3%. 

Zheng and Sun [67] used a thin-layer chromatographic method for the analysis of primaquine and other quinoline derivatives. The drug and other compounds were chromatographed on silica gel GF254 plate, with methanol aqueous 25 28% ammonia (200 3) and chloroform dichloromethane diethylamine (4 3 1), as mobile phases. Spots were located under ultraviolet radiation. The detection limit was 12 pg/mL. Total separation could be achieved by the use of two plates and the respective mobile phase. 

Although the detection of COads by in situ IR was accepted as not ruling out the existence of other adsorbed species (particularly since the experiments were not quantitative in terms of coverage and the potential-modulation aspect of the technique could render it blind to adsorbed species that do not exhibit a potential-dependent absorption frequency), it was generally accepted that the EMIRS data had ended the long controversy over the nature of the poison derived from methanol. 

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