TR201809158A2 - A METHOD FOR OBTAINING CAPSANOID AND ANALOGIES FROM PEPPER WASTE - Google Patents
A METHOD FOR OBTAINING CAPSANOID AND ANALOGIES FROM PEPPER WASTE Download PDFInfo
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- 235000002566 Capsicum Nutrition 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000006002 Pepper Substances 0.000 title claims abstract description 21
- 235000016761 Piper aduncum Nutrition 0.000 title claims abstract description 21
- 235000017804 Piper guineense Nutrition 0.000 title claims abstract description 21
- 235000008184 Piper nigrum Nutrition 0.000 title claims abstract description 21
- 239000002699 waste material Substances 0.000 title claims abstract description 17
- 244000203593 Piper nigrum Species 0.000 title abstract 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 48
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 28
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000284 extract Substances 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001704 evaporation Methods 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 239000003208 petroleum Substances 0.000 claims abstract description 7
- 239000000706 filtrate Substances 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 5
- YKPUWZUDDOIDPM-SOFGYWHQSA-N capsaicin Chemical compound COC1=CC(CNC(=O)CCCC\C=C\C(C)C)=CC=C1O YKPUWZUDDOIDPM-SOFGYWHQSA-N 0.000 claims description 48
- 229960002504 capsaicin Drugs 0.000 claims description 22
- 235000017663 capsaicin Nutrition 0.000 claims description 22
- 241000722363 Piper Species 0.000 claims description 20
- XJQPQKLURWNAAH-UHFFFAOYSA-N dihydrocapsaicin Chemical compound COC1=CC(CNC(=O)CCCCCCC(C)C)=CC=C1O XJQPQKLURWNAAH-UHFFFAOYSA-N 0.000 claims description 11
- RBCYRZPENADQGZ-UHFFFAOYSA-N dihydrocapsaicin Natural products COC1=CC(COC(=O)CCCCCCC(C)C)=CC=C1O RBCYRZPENADQGZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 7
- 238000000944 Soxhlet extraction Methods 0.000 claims description 6
- 240000004160 Capsicum annuum Species 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 235000002568 Capsicum frutescens Nutrition 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 235000008534 Capsicum annuum var annuum Nutrition 0.000 claims description 3
- 240000008574 Capsicum frutescens Species 0.000 claims 2
- 230000008020 evaporation Effects 0.000 abstract description 6
- 238000000605 extraction Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000003756 stirring Methods 0.000 abstract 1
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 12
- 150000001875 compounds Chemical class 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- 230000000975 bioactive effect Effects 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 239000007858 starting material Substances 0.000 description 6
- 244000185501 Capsicum chinense Species 0.000 description 5
- 241000758706 Piperaceae Species 0.000 description 5
- 239000008346 aqueous phase Substances 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 235000013399 edible fruits Nutrition 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical group CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 210000000056 organ Anatomy 0.000 description 3
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 235000002567 Capsicum annuum Nutrition 0.000 description 2
- 235000007862 Capsicum baccatum Nutrition 0.000 description 2
- 235000018306 Capsicum chinense Nutrition 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- 239000002154 agricultural waste Substances 0.000 description 2
- 239000001728 capsicum frutescens Substances 0.000 description 2
- 235000021466 carotenoid Nutrition 0.000 description 2
- 150000001747 carotenoids Chemical class 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 238000000622 liquid--liquid extraction Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 235000013311 vegetables Nutrition 0.000 description 2
- 241000208293 Capsicum Species 0.000 description 1
- 208000005156 Dehydration Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001851 biosynthetic effect Effects 0.000 description 1
- 239000001390 capsicum minimum Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000004807 localization Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002207 metabolite Substances 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000037361 pathway Effects 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 238000013379 physicochemical characterization Methods 0.000 description 1
- 210000002826 placenta Anatomy 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 235000019633 pungent taste Nutrition 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009885 systemic effect Effects 0.000 description 1
- 235000019640 taste Nutrition 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- Extraction Or Liquid Replacement (AREA)
- Seasonings (AREA)
Abstract
Buluş kapsanoid ve analoglarının eldesi ile ilgilidir. Geliştirilen yöntem, ekstraktlar biber atık kısmı olmak üzere; MeOH çözeltisi ile belirli bir süre boyunca soxhlet ekstraksiyonunun yapılması, aktif karbon ilavesi ile ekstraktların ısıtılarak karıştırılması, süzülmesi, aktif karbonun en az bir kez MeOH ile yıkanması, elde edilen süzüntünün kuruyana kadar evapore edilmesi, kalıntının petrol eteri ile çözülmesi, su ile yıkanması ve sulu tabakanın atılması, eter fazının kuruyana kadar evapore edilmesi ve kalıntının elde edilmesi işlem basamaklarını içermektedir.The invention relates to the production of capsanoids and analogs thereof. The developed method includes extracts of pepper waste; Extraction of soxhlet with MeOH solution for a certain period of time, stirring of the extracts by heating with the addition of activated carbon, filtration, washing of the activated carbon with MeOH at least once, evaporation of the resulting filtrate to dryness, washing of the residue with petroleum ether, washing with water and washing with water. layer removal, evaporation of the ether phase to dryness and obtaining the residue.
Description
TARIFNAME BIBER ATIKLARINDAN KAPSANOID VE ANALOGLARININ ELDE EDILMESI IÇIN BIR YÖNTEM Bulugun Konusu Bulus, farkli biber türlerinin yesil renkli bas kismi ya da sap kismi gibi atik kisimlarindan kapsanoid ve analoglarinin (dihidrokapsaisin ve kapsaisin) elde edilmesi için gelistirilen bir yönteme iliskindir. DESCRIPTION OBTAINING KAPSANOID AND ITS ANALOGUES FROM PEPPER WASTE A METHOD FOR Subject of the Finding The invention is the green-colored bass part of different pepper species or Capsanoid and its analogues from waste parts such as stem part (dihydrocapsaicin and capsaicin) to obtain relates to a developed method.
Teknigin Bilinen Durumu Kapsanoid ve analoglari olan dihidrokapsaisin ve kapsaisin, meyve ya da sebzelerden ticari olarak ya da bilimsel alanda kullanilmak üzere belirli saflik oranlarinda izole edilmektedir. Kapsaisin, biberin etken maddesi olup, bibere keskin yakici tadi vermektedir. Kapsaisin içeren biberin besinsel olarak tüketilmesinin yani sira, birçok farkli alanda kullanimi da mevcuttur. Örnek olarak kapsanoid ve analoglari ilaç ve kozmetik sektöründe etken madde olarak kullanilmaktadir. State of the Art Capsanoids and their analogues, dihydrocapsaicin and capsaicin, from fruit or vegetables commercially or scientifically isolated at certain purity ratios to be used is being done. Capsaicin is the active ingredient of pepper. It gives a sharp burning taste. Capsaicin-containing pepper In addition to being consumed nutritionally, many different It is also available for use in the field. For example, capsanoid and analogues as active ingredients in the pharmaceutical and cosmetic industry. is used.
Teknikte ticari olarak kullanilan kapsaisinin saflastirilmasina yönelik yöntemler mevcuttur. U5595563l sayili patent dokümani buna örnek olarak verilebilir. Capsaicin commercially used in the art There are methods for purification. U559563l The patent document no. is given as an example.
Bahsedilen dokümana konu saflastirma yöntemine göre elde edilen özütlerin her bir numunesi petri kabindan 30 ml aseton çözücüsüyle çözülüp alinmistir. Deney için 30 ml O,l M AgN03 çözeltisi eklenip 30°C' de pH 7 oluncaya kadar 0,1 M NAOH çözeltisi damla damla (yaklasik 3 damla) eklenmektedir. Sonra 3 saat boyunca manyetik karistiricida ekstraksiyon yapilir. The subject of the mentioned document is obtained according to the purification method. Each sample of the extracted extracts was removed from the petri dish with 30 ml of acetone. dissolved with solvent. 30 ml of 0.1 M AgNO3 for the experiment 0,1 M NAOH solution is added until the pH is 7 at 30°C. solution is added dropwise (approximately 3 drops). Then Extraction is done in magnetic stirrer for 3 hours.
Daha sonra çözelti dinlendirilir. Adi süzgeç kagidi ile süzülüp sulu faz ayrilir. Sulu faza 100 ml hekzan eklenerek sivi-sivi ekstraksiyon yapilir. Sulu faza 25 ml diklormetan eklenip sulu faz ayrildiktan sonra sulu faza 2. kez 25 ml diklormetan eklenir. Diklormetan fazlari toplanir ve yaklasik 50 ml olan çözelti rotary evaporatörde yarisi kalacak sekilde çözücüsü uçurulur. Kapsanoidleri içeren (hangi numuneden saflastirilacaksa) çözeltiye tekrar 25 ml doygun NaCl çözeltisiyle sivi-sivi ekstraksiyon gerçeklestirilir. The solution is then rested. With ordinary filter paper filtered and the aqueous phase separated. Adding 100 ml of hexane to the aqueous phase liquid-liquid extraction is done. 25 ml of dichloromethane to the aqueous phase After adding and separating the aqueous phase, 25 ml is added to the aqueous phase for the second time. dichloromethane is added. The dichloromethane phases are collected and approx. The solution of 50 ml should be left half in the rotary evaporator. solvent is evaporated. Containing capsanoids (from which sample if it is to be purified) add 25 ml of saturated NaCl again to the solution. Liquid-liquid extraction is performed with the solution.
Sonrasinda diklormetan fazi alinir ve çözücü uzaklastirilir. The dichloromethane phase is then removed and the solvent is removed.
Buna ek olarak, sebze ve meyvelerden elde edilen kapsaisinin, bu bitkilerin atigi olarak tanimlanan sekonder metabolitlerinden eldesine iliskin bazi çalismalar da teknikte mevcuttur. In addition, capsaicin from vegetables and fruits, secondary, defined as waste from these plants Some studies on the production of metabolites available in the art.
Teknigin bilinen durumuna örnek olarak ”Physicochemical characterization and bioactive compounds of stalk from hot fruits of Capsicumannuum L.” isimli makale verilebilir. As an example of the state of the art ”Physicochemical characterization and bioactive compounds of stalk from hot fruits of Capsicumannuum L.” article can be given.
Bahsedilen patent disi doküman, kirmizi aci biber sapinda bulunan besleyici ve uçucu bilesiklerin, biyoaktif kapsaisinin ve karotenoidlerin miktarinin belirlenmesine iliskindir. Dokümanda anlatilanlara göre; bunun için, 0.25 mm, 0.5 mm ve 1.0 mm parçacik boyutlarinda kirmizi aci biber (Capsicumannuum L.) sapinda, besleyici ve uçucu bilesiklerin, biyoaktif kapsaisin ve karotenoidlerin miktarlari belirlenmistir. Ayrica sap kismi, TGA, DSC ve FTIR spektroskopisi kullanilarak karakterize edilmistir. Protein, kül ve selülozun içerigine, parçacik büyüklügünün etkisi önemsiz olarak degerlendirilmistir. 0,5 ve 1,0 mm'ye kiyasla, 0.25 mm partikül boyutundaki sap, daha koyu sari-kahverengi bir renge sahip olup, mikro elementler açisindan daha zengindir. Yagi zengin, en yüksek ekstrakt miktari, etanol kullanilarak 0.25 mm partikül büyüklügünde saptan elde edilmistir. Kapsaisin ekstraksiyonu için de daha etkilidir. The aforementioned non-patent document is on the stalk of red hot pepper. nutrient and volatile compounds found in bioactive quantification of capsaicin and carotenoids is related. According to what is described in the document; for this, 0.25 Red hot pepper in particle sizes of mm, 0.5 mm and 1.0 mm (Capsicumannuum L.) sap, nutritive and volatile compounds, Quantities of bioactive capsaicin and carotenoids has not been determined. Also the handle part, TGA, DSC and FTIR characterized using spectroscopy. Protein, The effect of particle size on the content of ash and cellulose rated as unimportant. Compared to 0.5 and 1.0 mm, 0.25 mm particle size stalk, darker yellow-brown has a color and is more in terms of microelements. he is rich. Rich in oil, highest amount of extract, ethanol obtained from the stem with a particle size of 0.25 mm using has been made. It is also more effective for capsaicin extraction.
(CapsicumchinenseJacqç)”isimli makale de teknigin bilinen durumuna örnek olarak verilebilir. Söz konusu patent disi doküman, Habanero biberinin bitkisel organlarinda kapsaisinoid tayinine iliskindir. Dokümanda anlatilanlara göre; kapsaisinoidler, keskinlik Özelligini biberlere veren kimyasal bilesikler, Capsicum cinsinin tüm türlerinde farkli seviyelerde birikmektedir. Kapsaisinoid sentezinin, biber meyvelerinin plasenta interloçularseptumunda olustugunu gösteren birçok kanit vardir. Bununla birlikte, kapsaisinoid biyosentez birikim yollarinin kesin lokalizasyonu hala tartisilmaktadir. Bu nedenle, bu çalismanin amaci, biber bitkilerinin kapsaisinoid biyosentezinin sistemik regülasyonunu açikliga kavusturmak için dolayli bir yol olarak vejetatif organlarda kapsaisin sentezini ya da kapsaisinin› biriktirip birikmedigini degerlendirmektir. Bu amaçla dünya çapinda en aci biberlerden biri olan Yucatan Yarimadasi'nda yetisen habanero biberi incelenmistir. (CapsicumchinenseJacqç)” is also known in the article. situation as an example. The patent in question document, in vegetative organs of Habanero pepper It is related to the determination of capsaicinoid. to what is described in the document by; capsaicinoids, which give peppers their pungency chemical compounds differ in all species of the genus Capsicum. accumulating levels. Capsaicinoid synthesis, pepper that its fruits are formed in the placenta interlocular septum There is a lot of evidence that shows. However, capsaicinoid The precise localization of the biosynthetic accumulation pathways is still are discussed. Therefore, the aim of this study is to systemic effects of capsaicinoid biosynthesis an indirect way to clarify the regulation of Capsaicin synthesis in vegetative organs or is to evaluate whether capsaicin accumulates or not. This Yucatan, one of the hottest peppers worldwide, Habanero pepper grown in the peninsula has been studied.
Kromatografik ve enzimatik ölçümlerle elde edilen sonuçlar, habanero biber bitkilerinin, su stresi kosullarinda bile analiz edilen vejetatif organlarda kapsaisinoidlerin biriktirmedigine dair saglam kanitlar sunmaktadir. Results obtained by chromatographic and enzymatic measurements, of habanero pepper plants, even under water stress conditions. capsaicinoids in vegetative organs analyzed provides solid evidence that it does not accumulate.
Teknigin bilinen durumuna baska bir örnek olarak “Recovering Bioactive Compounds from Agricultural wastes” isimli makale verilebilir. Bahsedilen patent disi doküman, tarimsal atiklardan biyoaktif bilesik eldesine iliskindir. Ilgili dokümanin l99. sayfasinda biber atigindan biyoaktif birlesik üretimi anlatilmaktadir. Söz konusu kisma göre tarimsal atik ürün, yüksek fenolik, flavanoid ve kapsaisin içerigine sahip kirmizibiber sapidir. Dokümanda anlatilanlara göre; çogunlukla, kirmizibiber saplari karaya veya nehirlere atilir. Buralarda oksitlenerek lokal ekolojiye zarar vermektedir. Böylece, biber sapi atiklarini yeniden islemeye yönelik herhangi bir girisim yararli olarak düsünülmektedir. As another example of the state of the art, “Recovering Article titled “Bioactive Compounds from Agricultural wastes” can be given. The aforementioned non-patent document It is related to the production of bioactive compounds from wastes. Relating to l99 of the document. bioactive compound from pepper waste production is described. According to the said section, agricultural waste The product has high phenolic, flavonoid and capsaicin content. red pepper stalk. According to what is described in the document; often, red pepper stalks are washed ashore or into rivers. is discarded. Damage to local ecology by oxidizing here gives. Thus, to reprocess the pepper stalk waste. Any attempt at this is considered beneficial.
Bir geleneksel ekstraksiyon teknigi, çözücünün katidan sivi faza aktarilmasi için düsük basinçli kosullar altinda (0.1MPa'ya yakin oda basinci) organik çözücülerin kullanimini Yukarida bahsedilen biber atiklarindan kapsanoidlerin eldesine iliskin yapilan çalismalara alternatif olarak, farkli genotipte biberlerin yesil renkli bas kismi ya da sap kismi gibi atik kisimlarindan yüksek verimli olarak kapsanoid ve analoglarinin elde edilmesini saglayan bir izolasyon yöntemi gelistirilmistir. One traditional extraction technique is to remove the solvent from the solid to the liquid. under low-pressure conditions to transfer to phase (room pressure close to 0.1MPa) use of organic solvents Capsanoids from the aforementioned pepper wastes As an alternative to the studies on the green-colored head or stem of peppers of different genotypes high efficiency capsanoid from waste parts such as and an isolation that allows to obtain analogues method has been developed.
Bulusun Detayli Açiklamasi Bulus, farkli genotipte biberlerin atigi olarak tanimlanan sap ve bas kisimlarindan kapsanoid ve analoglarinin eldesi için bir yöntem sunmaktadir. Kapsanoid analoglari dihidrokapsaisin ve kapsaisin olarak tanimlanmaktadir. Detailed Description of the Invention The invention is defined as the waste of different genotype peppers. Obtaining capsanoid and its analogues from stem and bass parts It offers a method for Capsanoid analogs It is defined as dihydrocapsaicin and capsaicin.
Bulusa konu yöntem, farkli genotipteki biberlerin atik kisimlarini içeren ekstraktlara uygulanarak kapsanoid ve analoglarinin bilesik olarak elde edilmesini saglamaktadir. The method, which is the subject of the invention, is the waste of different genotype peppers. by applying to extracts containing parts of capsanoid and It enables the analogues to be obtained as compounds.
Bulusa konu yöntem en genel haliyle, biber atik kismindan elde edilen ekstraktlarin, MeOH çözeltisi ile belirli bir süre boyunca soxhlet ekstraksiyonunun yapilmasi, aktif karbon ilavesi ile ekstraktlarin isitilarak karistirilmasi, süzülmesi, aktif karbonun en az bir kez MeOH ile yikanmasi, elde edilen süzüntünün kuruyana kadar evapore edilmesi, kalintinin petrol eteri ile çözülmesi, sivi ile yikanmasi ve sivi tabakanin atilmasi, eter fazinin kuruyana kadar evapore edilmesi ve kalintinin elde edilmesi islem basamaklarini içermektedir. The method which is the subject of the invention, in its most general form, is obtained from the pepper waste part. The obtained extracts were mixed with MeOH solution to a certain extent. soxhlet extraction during the period, activated carbon mixing the extracts by heating with the addition of filtering, washing the activated carbon at least once with MeOH, evaporation of the filtrate obtained until it dries, dissolving the residue with petroleum ether, washing with liquid and removal of the liquid layer, evaporation of the ether phase until dry process steps of obtaining the residue and obtaining the residue contains.
Bulusun bir yapilandirmasinda ekstraktlar biber atigidir. In one embodiment of the invention, the extracts are pepper powder.
Bulusun bir yapilandirmasinda ekstraktlar biberin bas kismi ve/veya sap kismini içermektedir. In one embodiment of the invention, the extracts are the head of the pepper. and/or stem portion.
Bulusun bir yapilandirmasinda aktif karbon birkaç kez MeOH ile yikanmaktadir. Tercihen %100 MeOH ile yikanmaktadir. In one embodiment of the invention, the activated carbon is several times MeOH is washed with It is preferably washed with 100% MeOH.
Bulusun bir yapilandirmasinda, kalintinin yikanmasi için sivi olarak su kullanilmaktadir. Kapsaisin ve türevlerinin suda çözünürlügünün oldukça düsük olmasindan dolayi, su ile safsizligin giderilmesi amaçlanmaktadir. Buna ek olarak maliyet açisindan su uygun bir çözücüdür. In one embodiment of the invention, the liquid for washing the residue water is used. Capsaicin and its derivatives in water Due to its very low solubility, it can be mixed with water. It is aimed to remove the impurity. In addition In terms of cost, water is a suitable solvent.
Bulusun bir yapilandirmasinda kalinti, petrol eteri ile çözüldükten sonra ayirma hunisinde su ile yikanmaktadir. In one embodiment of the invention, the residue is mixed with petroleum ether. After dissolving, it is washed with water in a separating funnel.
Bulusun bir yapilandirmasinda soxhlet ekstraksiyonu 200 ml MeOH çözeltisi ile 24 saat boyunca yapilmaktadir. Soxhlet extraction in one embodiment of the invention 200 ml It is done with MeOH solution for 24 hours.
Bulusun bir yapilandirmasinda soxhlet ekstraksiyonu 20 g kati madde basina en az 200 ml %100 MeOH çözeltisi ile en az 24 saat boyunca yapilmaktadir. In one embodiment of the invention, soxhlet extraction 20 g solid At least 24 hours with at least 200 ml of 100% MeOH solution per substance is done around the clock.
Bulusun bir yapilandirmasinda 1 g aktif karbonun 10 dakika boyunca ilave edilmesi suretiyle ekstraktlar isitilarak karistirilmaktadir. In one embodiment of the invention, 1 g of activated carbon is used for 10 minutes. by heating the extracts by adding are mixed.
Bulusun bir yapilandirmasinda gelistirilen yöntenu 200 ml ekstraksiyonunun yapilmasi, 10 dakika boyunca 1 g aktif karbon ilavesi ile ekstraktlarin isitilarak karistirilmasi, süzülmesi, aktif karbonun birkaç kez %100 MeOH ile yikanmasi, elde edilen süzüntünün kuruyana kadar evapore edilmesi, kalintinin petrol eteri ile çözülmesi, ayirma hunisinde su ile yikanmasi ve sulu tabakanin atilmasi, eter fazinin kuruyana kadar evapore edilmesi, kalintinin elde edilmesi islem basamaklarini içermektedir. The method developed in one embodiment of the invention is 200 ml extraction, 1 g of activated carbon for 10 minutes mixing the extracts by heating with the addition of filtering, washing the activated carbon several times with 100% MeOH, evaporation of the filtrate obtained until it dries, dissolving the residue with petroleum ether, water in the separatory funnel and removal of the aqueous layer, the ether phase evaporation until dry, obtaining the residue contains the steps.
Bulusun yapilandirmalari ile kapsanoid ve analoglari (dihidrokapsaisin ve kapsaisin), biber atik numunelerinden izole edilmektedir. Capsanoid and analogs with embodiments of the invention (dihydrocapsaicin and capsaicin), from pepper waste samples is isolated.
Bulusun bir yapilandirmasinda analitik prosedür su sekilde açiklanmaktadir: Bulusun yukarida anlatilan yapilandirmalarindan birinde elde edilen kalinti lOmL MeOH ile viallenir. HPLC sisteminde ODS- olup mobil faz Asetonitril / Su (pz30) izokratikolarak UV-Vis detektör ile 230 ve 280 nm dalga boyunda analiz gerçeklestirilir. Analiz metodu 10 dakika olup enjeksiyon hacmi 20 mikrolitredir. In one embodiment of the invention, the analytical procedure is as follows: explains: achieved in one of the above-described embodiments of the invention. The resulting residue is vial with 10mL of MeOH. ODS- in HPLC system and the mobile phase is Acetonitrile / Water (pz30) isocratic to UV-Vis. Analysis with detector at 230 and 280 nm wavelengths is performed. The analysis method is 10 minutes and injection. Its volume is 20 microliters.
Gelistirilen yöntemde kapsaisin, dihidrokapsaisin ve kapsanoid bilesik olarak elde edilmektedir. Bulusa konu yöntem uygulanmasi suretiyle kapsaisin, dihidrokapsaisin ve kapsanoid bilesenleri dört farkli biber atigi numunelerinden tek tek saflastirilmis, miktar tayini yapilmistir. Söz konusu farkli biber atiklarina iliskin miktar tayinleri asagida belirtilmektedir. In the developed method, capsaicin, dihydrocapsaicin and obtained as a capsanoid compound. subject of the invention capsaicin, dihydrocapsaicin and The capsanoid components were obtained from four different pepper powder samples. They were purified one by one and quantified. Aforementioned Quantitative determinations of different pepper wastes are given below. is indicated.
Numune 1: Kirmizi Aci Biber - 10 ml olarak viallenen numune 50.86868ppm olarak tespit edilmistir. ppm=mg/L olmakta ve 50 ppm = mg/(0,01 L) bulunmaktadir. - 3,4614 g baslangiç maddesinin. % 0,014`ü kapsaisin içermektedir. 3,4614 g baslangiç maddesinin % 0,016'si dihidrokapsaisin içermektedir. 3,4614 g baslangiç maddesinin % 0,030'u toplam kapsanoid içermektedir. Sample 1: Red Hot Pepper - The sample vialed as 10 ml is determined as 50.86868ppm has been made. ppm = mg/L and 50 ppm = mg/(0.01 L) are available. - 3.4614 g of starting material. 0.014% capsaicin contains. 0.016% of 3.4614 g starting material dihydrocapsaicin contains. 0.030% total capsanoids of 3.4614 g starting material contains.
Numune 2: Aci Samandag - 10 ml olarak Viallenen numune 95.83977ppm olarak tespit edilmistir. ppm=mg/L olmakta ve 95ppm = mg/(0,0l kapsaisin bulunmaktadir. - 1,7522 g baslangiç maddesinin % 0,057`si kapsaisin içermektedir. 1,7522 g baslangiç maddesinin % 0,033'ü dihidrokapsaisin içermektedir. 1,7522 g baslangiç maddesinin % 0,090'ni toplam kapsanoid içermektedir. Sample 2: Aci Samandag - Vialed sample as 10 ml was determined as 95.83977ppm has been made. ppm=mg/L and 95ppm = mg/(0.0l contains capsaicin. - 0.057% of 1.7522 g starting material capsaicin contains. 0.033% of 1.7522 g starting material dihydrocapsaicin contains. Total capsanoids constitute 0.090% of 1.7522 g starting material contains.
Numune 3: Kirmizi Tatli Biber - 10 ml olarak viallenen numune 0.38100ppm. olarak tespit edilmistir. ppm=mg/L olmakta ve0,38l ppm = mg/(0,0l bulunmaktadir. içermektedir. içermektedir. kapsanoid içermektedir. Sample 3: Red Sweet Pepper - The sample vialed as 10 ml is 0.38100ppm. detected as has been made. ppm=mg/L and 0.38l ppm = mg/(0.0l are available. contains. contains. Contains capsanoids.
Numune 4: Yesil Apras Aci Biber - 10 nü_ olarak 'viallenen numune 8.64513ppm. olarak tespit edilmistir. ppm=mg/L olmakta ve 8.64513ppm = ng/(0,01 L) bulunmaktadir. içermektedir. içermektedir. içermektedir. Sample 4: Green Apras Hot Pepper - Vialized sample 8.64513ppm as 10 nubs. detected as has been made. ppm = mg/L and 8.64513ppm = ng/(0.01 L) are available. contains. contains. contains.
Bulus, literatürde tanimlanan kapsaisin eldesi için kullanilan mevcut yöntemlerden farkli bir prosedür ile uygulanan bir izolasyon yöntemi sunmaktadir. Bulus sayesinde milyonlarca ton biber atigi olarak açiga çikan biberin sap ve bas kisimlarindan kapsanoid. ve analoglari saflastirilmis, miktar ve tayini gerçeklestirilmistir. The invention is used to obtain capsaicin described in the literature. with a procedure different from the existing methods used presents an applied isolation method. Thanks to the invention The stem and stem of the pepper, which is released as millions of tons of pepper waste, capsanoid from bass parts. and its analogs purified, quantity and determination has been made.
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