Opium residues

The estimation of thebaine in the analysis of opium is described by Klyachkina [55] and Anneler [56], The alkaloid has been estimated in opium residues by condensation with benzoquinone, isolation of the very sparingly soluble adduct, and iodimetric titration of this in chloroform solution. This method is reported to be accurate to 0-5 per cent., provided resins, dyeing substances, and phenolic alkaloids are first removed [57]. Thebaine can also be estimated as its silicotungstate [53] or salicylate [54]. 

The thebaine content of opium residues has been determined by treatment of the residues with benzoquinone, isolation of the adduct, and iodimetric titration of the latter in chloroform [7]. 

Studies on risk factors for oesophageal cancer in the Caspian littoral of Iran carried out by lARC confirmed that the factors associated with the very high morbidity in this area included nutritional deficiencies and the chewing of the opium residues (dross or sukteh) from pipes or inhaled as opium smoke (Ghadirian et al. 1985). 

Noscapine [128-62-1] (45) is the second most abundant alkaloid found in opium. Unlike most opium alkaloids, however, it has an isoquinoline rather than a phenanthrene ting system. Noscapine was first isolated in 1817 but its antitussive activity was not demonstrated pharmacologically until 1952 (63). Clinical studies have confirmed its effectiveness. It is not a narcotic and has a wide margin of safety when given orally. Death could be produced in rats only with doses > 800 mg/kg (64). Noscapine is isolated from the water-insoluble residue remaining after processing opium for the manufacture of morphine. 

The large scale on which morphine is manufactured has made it possible to conduct investigations on practically unlimited supplies of factory residues, with the result that many alkaloids have been isolated from opium, of which at present twenty-five are known. In the following table, giving their names and formulae, they have been divided into five groups —... 

Mohn-saft, OT. poppy juice, opium, -samen, ot. poppyseed, -saure,/. meconic acid, -stoff, m. narcotine, -stroh, n. lit., poppy straw (residue from extraction of poppy heads and stems). 

Meconin is a neutral, non-nitrogenous body, which does not form salts. It is prepared by exhausting powdered Smyrna opium with boiling ether. The residue, after distilling off the ethcT, is repeatedly boiled with water,the solution evaporated,the residue dissolved in ether, decolorized with animal charcoal, evaporated, and the meconia obtained reorystallizod from water. 

DROSS The residue remaining in the pipe after prepared opium has been smoked. 

Flavoring substances can also be added to opium, including spices, sugar, and/or honey to disguise its bitter taste. It is also mixed into opium wine mixtures, some of which are called Yen Shee Suey. Dross, the residue remaining in the pipe after prepared opium has been smoked, may be mixed with raw opium. Re-using this dross is a cost-cutting measure in opium production. 

To Test tho Purity of Opium. Macerate 100 grains opium for 24 hours in 2 fluid ounces water filter and express the residue then precipitate with a solution of onneo carbonate of soda in 2 fluid ounces cold water gently heat tho precipitate until it fuses, then cool and weigli it. It should wcigli at least 10 grains and, when powdered, bo entirely soluble iu a solution of oxalic ncid. 

The isolation of narcotine from opium is simplified by the fact that most of it remains in the water-insoluble residue when opium is processed for the manufacture of morphine. The narcotine is then extractable from this residue with dilute acids, and after regeneration from the extract it may be purified by recrystallization from ethanol (107). The acid oxalate, m.p. 174°, has also been used to separate it from its chief contaminant, namely, papaverine (92,108, 109). Its salt with camphorsulfonic acid is practically insoluble in water whereas that of the other opium salts are quite soluble (110). The free base may be quickly purified by passing a chloroform or benzene solution through a column of calcium hydroxide, most of the impurities being absorbed (HI). 

In yet another method, Ono et al. (1977, 1978) separated opium alkaloids on a silicone OV-1 column as follows after triturating with 1% HCl, opium was filtered and extracted with CHCI3. The CHCI3 extract was treated with NH3, evaporated and dissolved in acetone, and injected in gas chromatograph for thebaine, papaverine, and noscapine determination. The aqueous acidic layer was neutralized with NH3 and extracted with CHCl3-iso-PrOH (3 1) mixture, evaporated, and the residue was treated with bistrimethylsilylacetamide at 90 °C for 10 min. Codeine and morphine were then determined by gas chromatography. 

The name alcaloide is used by Dumas as an alternative to the alcalis veg taux of Berzelius. C. L. Derosne on diluting an evaporated extract of opium obtained a crystalline precipitate, which he recrystallised from alcohol. He found that the extract of opium is precipitated by alkali and the crystalline precipitate, even after washing, turned syrup of violets green, which he supposed was due to residual alkali, and since the first preparation did not he regarded it as a salt-like substance. Derosne concluded that opium contains a peculiar acid salt . He showed that the preparation had the same narcotic properties as a larger quantity of opium. 

A purity assay of morphine is based on a similar reaction. Morphine base is contained in opium as a salt of meconic acid. Purified morphine in the presence of FeCH in hydrochloric acid must not give a red color. Meconic acid indeed yields a red color with Fe +. The presence of residual meconic acid is a mark of insufficient purification. The reaction of meconic acid with Fe + is... 

Mix intimately 1 g of sample with 0 25 g of slaked lime in a glass mortar. Add water gradually and transfer quantitatively to a 100-ml graduated flask. Shake the mixture (approximately 90 ml) frequently during thirty minutes, make up to 100 ml, shake and filter. To 10 ml of filtrate add 015 g of ammonium sulphate and continue the nitroso-morphine colorimetric assay as given under Camphorated Tincture of Opium except that the residue is dissolved in 5 ml of N hydrochloric acid and diluted to 50 ml. 20 ml of this solution is used for the colorimetric assay. 

Weigh 4 g into a small dish and evaporate the volatile solvents on a water-bath. Triturate the residue with 1 ml of dilute ammonia solution until a smooth cream is obtained and continue as described above for Camphorated Tincture of Opium beginning with the words add chromatographic aluminium oxide. . . and ending with the words. to about 1-5 ml per minute by means of gentle suction. Extract the morphine from the eluate with 10, 10 and 5 ml of 2 per cent w/v sulphuric acid solution, combine the extracts in another separator and make alkaline to litmus paper with dilute ammonia solution. Complete by the method for Mixture of Ammonium Chloride and Morphine from the words shake vigorously for two to three minutes. . . , but dissolve the residue in exactly 5 ml of 0-5N hydrochloric acid and dilute with water to 50 ml. Use 10 ml of this solution for application of the iodic acid-nickel chloride reaction described above. 

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