Drug – bio-affecting and body treating compositions – Antigen – epitope – or other immunospecific immunoeffector – Conjugate or complex
Patent
1986-07-24
1989-04-11
Rollins, John W.
Drug, bio-affecting and body treating compositions
Antigen, epitope, or other immunospecific immunoeffector
Conjugate or complex
424DIG10, A01K 6500
Patent
active
048205176
DESCRIPTION:
BRIEF SUMMARY
Ordinary commercial insecticides based on synthetic chemicals to be sure are effective, but because of their synthetic origin they are increasingly encountering objections among broad sectors of the population. Therefore, natural plant constituents with insecticidal activity are finding increasing interest. The best known example of this is pyrethrum, from Chrysanthemum cinerariaefolium.
Recently it was also found and described that black pepper or an extract of this shows toxic activity against a large number of insects. At first it was suggested that the sharp tasting principle of pepper, piperine or a derivative of piperine, should be considered responsible for the insecticidal activity. In later studies, however, it was shown that it is not piperine but rather other alkaloids of pepper which have insecticidal activity [Su and Horvat, Agricult. Food Chem., Vol. 29, p. 115, 1981]. The authors mentioned extracted ground black pepper with acetone and isolated alkaloids containing amide groups and having insecticidal activity from the extract with the aid of chromatographic methods. Black pepper is the dried, unripe fruit of the tropical plant, Piper nigrum L. and contains about 5-10% piperine as well as other sharp tasting alkaloids, 1-2.5% essential oils, and smaller amounts of other alkaloids which are not among the sharp tasting substances.
In addition, spices such as black pepper have already had their flavoring component removed with supercritical gas in terms of temperature and pressure, e.g., CO.sub.2, and the extract separated by changing the pressure or temperature (German Preliminary Published Application No. 2,127,611). Spice extracts, e.g., from black pepper, can also be obtained by withdrawing the essential oil acting as a flavor component in a first step with liquid subcritical CO.sub.2, and removing the fractions serving as the flavor carrier in a second step with supercritical CO.sub.2, separating the extracts by pressure and temperature alterations, and possibly mixing them together (European Patent No. 23,680). In both cases, however, the goal of this process is not directed toward obtaining insecticidally active extracts from black pepper, but rather at the manufacture of scenting or flavoring materials for the food or cosmetic industry.
It has now been found that a non-sharp-tasting fraction bearing insecticidal activity can be extracted from black pepper with compressed CO.sub.2 and obtained in pure form under suitable process conditions. In this extraction and recovery process attention is to be paid to the fact that the sharp tasting components, especially the piperine, are not also enriched or separated during the process sequence, since these can lead to mucous membrane irritations during the use of the insecticidal agent in the case of people who intentionally or unavoidably come into contact with the agent. Such an extraction and recovery process must also be economical and able to be carried out in the simplest possible way.
The subject of the invention is a process for obtaining a pepper extract with insecticidal activity, characterized by the following process steps:
(a) extraction of black pepper in ground form with CO.sub.2 at 30.degree.-70.degree. C. and 150-500 bar,
(b) separation of the sharp tasting fractions in a first expansion step at 25.degree.-35.degree. C. and 70-150 bar,
(c) removal of an oily fraction which contains the insecticidally active components as well as most of the essential oils, in a second expansion step at 15.degree.-30.degree. C. and 40-70 bar,
(d) obtaining the insecticidally active components by removing the essential oils by steam distillation.
The process can also be carried out by performing the extraction of the black pepper corresponding to the conditions of step (b) with CO.sub.2 at 25.degree.-35.degree. C. and 70-150 bar and separating from this by expansion at 15.degree.-30.degree. C. and 40-70 bar according to step (c) an oily fraction, which is further treated according to (d). In this case the sharp tasting components are left behind i
REFERENCES:
patent: 4123559 (1978-10-01), Vitzthum et al.
patent: 4198432 (1980-04-01), Vitzthum et al.
patent: 4490398 (1984-12-01), Behr et al.
Agricultural and Food Chemistry 1981, 29,115.
Biermann Manfred
Goebel Gerd
Mueller Annemarie
Pfeiffer Hans
Schroeder Peter
Henkel Kommanditgesellschaft auf Aktien
Jaeschke Wayne C.
Millson Jr. Henry E.
Rollins John W.
Szoke Ernest G.
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