Alkaloids detection

Sonnenschein s reagent (alkaloid detection) a nitric acid solution of ammonium molybdate is treated with phosphoric acid. The precipitate so produced is washed and boiled with aqua regia... 

Lawson, G., Ostah, N., and Woolley, J.G., MS/MS smdies of tropane alkaloids Detection and determination of stmctnre, m Applications of Modem Mass Spectrometry in Plant Science Research, Newton, R.P. and Walton, T.J., Eds., Clarendon Press, New York, 1996, chap. 16. 

Compounds Sample Plate Eluent Alkaloids Detection Remarks Reference... 

These analytical dilemmas interfere with the methods of alkaloid analysis. Each group of alkaloids has its own methods of extraction, isolation and crystallization, as well as detection in structure, molecule and dynamicity. Not all these stages are still possible in the majority of alkaloids. In recent years, many techniques have been used in alkaloid detection. There are atomic and molecular electronic spectroscopy, vibration spectroscopy and electron and nuclear spin orientation in magnetic fields, mass spectroscopy, chromatography, radioisotope and electrochemical techniques. Although important developments in methodology and... 

Gas-liquid chromatography is a qualitative, but also quantitative, method of alkaloid analysis. It is very sensitive. The only problem concerns the distribution of the alkaloid mixture in the chromatographic process and the identification of alkaloids, which must be achieved by a different technique . A very positive characteristic is the possibility of totally computerizing this method of alkaloid detection. 

Alkaloid isolation and structural elucidation is summarized in Table 6. In addition to known constituents, codeine and neopine have been isolated from Papaver brac-teatum Although callus cells from this plant contain thebaine at early stages of subculturing, only traces are found later. - ° Thebaine was identified among seventeen isoquinoline alkaloids detected in, or isolated from P. syriacum. ... 

Emetine,Cinchona alkaloids, Detection with conduc-scopolamine,brucine,strych- tance detector nine,reserpi ne,yohi mbi ne, caffeine Silica gel 10 jn CHC13-MeOH-hexane(7 3 10) 16... 

Additional 2,6-disubstituted piperidine alkaloids detected in Picea and Pinus include pinidinone and epipinidinone (191 and 194, from Picea pungens), 193 (from Picea abies, P. pungens), 195 (from Pinus nigra, P. sylvestris, P. ponderosa) and 196 (from Picea pungens, Pinus ponderosa, P. sylvestris, P. nigra)[467]. Pinidinone, an alcohol from reduction of pinidinone, and 196 have also been detected in the Mexican Bean Beetle, Epilachna varivestis [468]. 

The bark of Tecoma arequipensis (Bignoniaceae) yielded a major alkaloid, (-)-S-A-nor-methylskytanthine (32), [a]D -21.5°, whose structure was established through X-ray crystallographic analysis of the N-(4-bromophenylthiourea) derivative (36). Other alkaloids detected by GC-MS analysis included 5,6-dehydroskytanthine, skytanthine, actinidine, 5-hydroxy-skytanthine and tecomanine. Additional components were partially characterized (MS data only) as two hydroxytecomanines and four... 

Alkaloids Detected by Picric Acid. Hager has facid precipitates various alkaloids from their solutions, such as brucine, strychnine, veratrine, quinine, cinchonine, and some alkaloids of opium. Morphine and atropine, however, are precipitated only from neutral and concentrated sol a lions, d the precipitate dissolves pretty easily in water, Glucosides, casein, and pseudo-morphine resist the action of tho picric acid. 

This is the traditional method for alkaloid detection although care should be taken as some nonalkaloids such as iridoids and some flavonoids give a positive reaction Alkaloids give a dark orange-to-red coloration. 

Biemann and co-workers (114) have investigated the alkaloids of A. neblinae by combination gas chromatography-mass spectrometry. The alkaloids detected were aspidospermidine (249), 1,2-dehydroaspidosper-midine (171), deacetylpyrifolidine (250), 1,2-dehydrodeacetylpyrifolidine (251), JV-acetylaspidospermidine (252), aspidospermine (253), demethyl-aspidospermine (254), pyrifolidine (255), aspidocarpine (256), ebur-namonine (257), and neblinine (258). Both the power and the limitations of the technique are evident here. The technique is powerful in the sense that identification of microgram quantities of an alkaloid is easily made with computerized comparison of mass spectra. It has limitations, however, because compounds which are not stable to 300° (injector temperature) either will not be detected or will give alternate compounds, and that isolation must be made if the taxonomically important optical rotations of the alkaloids are to be determined. 

Alkaloids in bark (0.58%) and leaves (0.70% Preliminary characterization of a new alkaloid described Tertiary alkaloids detected Inhibitory action on muscle correlates with alkaloid content... 

Table 8-9. Acetylation products of the opioids and opium alkaloids detectable in urine...

A very positive characteristic is the possibility of totally computerizing this method of alkaloid detection. 

Aliquot of 2 mL is ready for alkaloid detection by the equipment to be prepared. 

For the purpose of the alkaloid detection by HPLC, the following protocol of extraction has been used by LopezAvila, Benedicto, and Robaugh. Extraction was done by the use of supercritical carbon dioxide alone and with supercritical carbon dioxide modified with 10% methanol. The methanol was exactly the same as used in the HPLC. The following steps are done ... 

Kursinszki et al. [36] have found that D. innoxia and A. belladonna hairy root cultures behaved in a similar way to Argentinean B. Candida hairy roots. In these cultures 6P-hydroxyhyoscyamine was also the predominant alkaloid detected [27, 36]. 

To determine the concentrations of vapor phase alkaloids detected in ETS by APCI mass spectrometry, it is necessary to have vapor phase standards which can be used for instrument calibration. Gas dilution is perhaps the best way to calibrate for compounds in the gas phase. Gas dilution requires that a standard of known concentration and a method for accurately and reproducibly diluting the standard are available. Permeation tubes and diffusion tubes, housed in a constant temperature oven, are well suited for generating gas standards with known analyte concentrations. Table 1 includes the analyte, source, and typical source effusion rates used for investigating ETS along with the ion monitored for quantitative analysis of each analyte. 

Fig. 11.27 (a-m) HPLC-MS/MS product ion spectra of alkaloids detected in the extract of the herb of Lobelia inflata cultivated in the field... 

The principal group of chemical compounds present in Aconitum species consists of diterpenoid alkaloids, detected in all parts of the plant. The maximal accumulation of alkaloids is observed in tubers. Other chemical substances found in plant are flavonol and kaempferol glycosides detected in aerial parts [15-17],... 

Table 3.4 Alkaloid profiles in the genus Nicotiana based on data from studies of Saitoh et aL (1985) as wen as Sisson and Severson (1990), updated according to the classification of Knapp et aL (2004). However - for direct compeuison with the original reports - sections and species in the order used by Saitoh et til. or by Sisson and Severson, i.e., not alphabetictilly like Knapp et al. ++ = Principal alkaloid detected by GC + = minor alkaloid detected by GC - not detected by GC...

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