PROCESS OF MAKING CURCUMINOID EXTRACT FROM TURMERIC RHIZOME (Curcuma longa)

Abstract

This invention relates to the process of making curcuminoid extract from turmeric rhizome (Curcuma domestica) using readily available, inexpensive, and safe solvents. This method is simple, easy, and fast to implement, and yields a large amount of yield. The steps taken in this process are sample preparation and curcuminoid extraction. Turmeric rhizomes are washed thoroughly with water, then peeled, sliced ​​thinly, then dried and made into powder. Turmeric rhizome powder is extracted solid-liquid using ethanol solvent. The extraction results are evaporated until a thick extract is formed. The resulting thick extract is extracted liquid-liquid using n-hexane solvent. The resulting extract contains curcuminoids in the ethanol phase, then evaporated until a yellow-orange powder is obtained. The curcuminoid components obtained are: curcumin, desmethoxycurcumin, and bisdesmethoxycurcumin.

Description

PROCESS OF MAKING CURCUMINOID EXTRACT FROM TURMERIC RHIZOME (Curcuma longa) Invention Engineering Field This invention concerns a process for making an extract curcuminoids from turmeric rhizomes (Curcuma longa) more specifically again, this invention relates to the process of making extracts curcuminoids from turmeric rhizomes using solvents ethanol 968 and n-hexane through soxhlet extraction and solvent extraction. The final result obtained is an extract curcuminoids in powder form in large quantities, the results characterization has been in accordance with the standard curcumin, namely consists of curcumin, desmethoxycurcumin, and bisdesmethoxycurcumin. Background of the Invention Curcuminoids are generally called curcumin. known and used for chemopreventive agents as well as anticancer agents potential therapy for several chronic diseases (Priyadarsini, 2014). Curcuminoids are reported to have various biological and pharmacological properties including anti-inflammatory activity oxidant, anti-inflammatory, anti-mutagenic, and anti-cancer (Anand et al., 2008: Kumar et al., 2016). Clinical studies that have been conducted in humans showing that curcuminoids very safe to use as a medicine even at high doses high with few side effects (Goel et al., 2008). The antioxidant activity of curcuminoids is very strong because its ability to catalyze the release of superoxide anions into hydrogen peroxide and oxygen in oxygen species reactive oxygen species (ROS) (Indira, 1997). Curcuminoids are components the largest of the turmeric that grows in tropical and subtropical areas especially in India and China. Turmeric has been used for centuries for the traditional treatment of various diseases, such as toothache, chest pain, and menstrual difficulties (Aggarwal et al., 2006). Due to the many benefits of curcuminoid compounds for health, as well as plant sources abundant turmeric, this compound has attracted attention so that an extraction method is needed that is easy, cheap and efficient. Technological inventions related to extraction curcuminoids from turmeric have also been described as contained in patent number CN107715052A dated 02-23-2018 with the title Method for extracting curcuma oil and total curcumin in Curcuma longa as well as applications thereof where it is stated that extraction is carried out using several organic solvents which are then separated using alumina column chromatography using gradient eluent based on the polarity of the solvent, but the invention is still there are drawbacks because various types of solvents are needed with different polarities with long steps for obtaining curcumin. Other inventions as disclosed on patent number CN1159741667A dated 04-18-2023 with the title Curcumin extraction method which is expressed in the extraction using microwaves, using a pulsed electric field high voltage bipolar square wave. However the invention mentioned above still has weaknesses weaknesses and limitations which include those required equipment that is not generally available, complicated separation stages, there are many steps to be taken, and expertise is required in the operation of the tool. Furthermore, the proposed invention This is intended to address the issues raised above by means of extraction quickly, easily, using solvents and equipment that are easy to obtain but have high yield. Brief Description of the Invention The object of the first invention is to disclose a process production of curcuminoid extract from turmeric rhizome (Curcuma longa) with the following steps 1. Process of making curcuminoid extract from turmeric rhizome (Curcuma longa) with the following steps a. 40 grams of turmeric rhizome powder was extracted with Soxhletation method using 250 ml of ethanol 968 temperature 75-85”C: b. The results of the extraction stage a are evaporated using rotary evaporation. Vacuum evaporator or evaporated over a water bath at a temperature 40-50”C until a thick extract of 50 ml is formed Cc. The resulting thick extract stage b was carried out liquid-liquid extraction using n-hexane solvent with The 1:1 ratio is repeated until the n-hexane phase is reached. colorless three times: d. The extract produced in stage c. which contains Curcumin in ethanol is evaporated with a water bath at a temperature of 40- 509C until a yellow-orange powder is obtained yield of more than 0.4% of the weight of wet turmeric or more of 28 weight of dry turmeric powder 2. The process of making curcuminoid extract from turmeric rhizomes (Curcuma longa) according to claim 1, wherein in year c is carried out further shaking using a separating funnel with combination of ethanol 968 and n-hexane solvents with a ratio of 1:1, Brief Description of the Invention Drawings Figure 1, is a flow diagram of curcuminoid extraction from turmeric rhizome Figure 2 is the UV-Vis spectrum of the extracted curcuminoids. Figure 3 is the UV-Vis spectrum of Merck standard curcumin. Figure 4 is the FTIR spectrum of the extracted curcuminoids. Figure 5 is the FTIR spectrum of Merck standard curcumin. Complete Description of the Invention The main objective of this invention is to overcome pre-existing problems, especially the process production of curcuminoid extract from turmeric rhizome (Curcuma longa. Curcuminoids are yellow-orange pigments, which are compounds widely studied natural phenomenon that has been shown enormous potential for in vitro therapy. For centuries centuries, has been used in Ayurvedic medicine and herbal medicine traditional Chinese medicine. Curcuminoids have been found to have pleiotropic activity due to its potential. This polyphenol is for modulate several signaling molecules. Curcuminoids exhibits anti-inflammatory, antioxidant, proapoptotic effects, chemopreventive, chemotherapy, antinociceptive, antiproliferative, antiparasitic, and antimalarial, and is used as an agent wound healing. Research on curcumin and its activity its pharmacology has become increasingly important in several last year (Urocevic et al., 2022). Curcuminoids give the powder its yellow-orange color. turmeric due to the extensive electronic delocalization within molecules that show strong absorption between 420 to 430 nm in organic solvents. Curcuminoids are a mixture curcumin, which is chemically diferuloylmethane (1,7!- bis(4-hydroxy-3-methoxy-phenyl)-hepta-l, 6-diene-3, 5-dione| which is mixed with two of its derivatives, namely demethoxycurcumin (4-hydroxycinnamoyl-(4-hydroxy-3-methoxycinnamoyl) methane | and bisdemethoxycurcumin (bis-(4-hydroxy cinnamoyl) methane | (Amalraj et. al, 2017). Although the extraction and separation of curcumin from the powder turmeric has been reported since 1815, the extraction method better results are still being reported. Solvent extraction is followed by with column chromatography is the most common method used to separate curcumin from turmeric, and some polar and non-polar organic solvents have been used, including hexane, ethyl acetate, acetone, methanol, etc. From solvents organic solvents used, ethanol has been found to be a solvent the most preferred for extracting curcumin (Priyadarsini, 2014). Extraction is the process of separating materials from the mixture using a suitable solvent. The process extraction is stopped when equilibrium is reached between concentration of compound in solvent with concentration in cell plants, in this case the extraction of curcuminoids from turmeric. In the extraction process according to the present invention there is two types of extraction, namely solid-liquid extraction using Soxhlet apparatus and liquid-liquid extraction (solvent extraction) using a separating funnel. Solid-liquid extraction according to This invention uses ethanol as a solvent, because this solvent This provides the best solubility of curcuminoid compounds. Soxhletation is a process to separate a components of a solid using a solvent volatile liquid. A number of samples will be extracted the active substance is wrapped in filter paper in the form of a lead. In the Soxhlet flask the solvent will be heated with using the appropriate boiling point until it evaporates, through The steam condenser will condense and drip onto the material or sample. is on the lead. When the solvent has soaked the material or the sample and solvent have exceeded the height of the flow pipe then The extract will flow again towards the Soxhlet flask. The extract reheated so that the solvent will evaporate and the substance extracted will be left in the Soxhlet flask. On this principle there will be a new recycling process where every time the material extracted then it will be extracted with a new solvent. The advantage of this extraction is that the active compounds are extracted directly. maximum and efficient use of solvents. Liquid-liquid extraction, or solvent extraction is the process of separating a component from a mixture based on distribution process of two types of solvents that are not mutually exclusive mixed. This separation can be done both at the macro level or micro. The principle of this method is based on the distribution of substances dissolved in a certain ratio between two immiscible solvents miscible with each other, such as benzene, n-hexane, petroleum ether, chloroform, and so on. Extraction can be done by continuous or gradual, gradual extraction is sufficient with a separating funnel. The mixture of two solvents is introduced with separating funnel, layer with lighter specific gravity is on the top layer. According to invention 1InNni, a process for making an extract curcuminoids from turmeric rhizomes (Curcuma longa) consist of Sample preparation stages and extraction process as follows. 1. Wash the turmeric rhizome thoroughly with water to remove any dirt. in the form of soil removed including the roots accompanying it. Roughly peeled turmeric does not have to be completely clean from the skin, then slice thinly diagonally, then oven at a temperature of 50-110°C until dry with Check the hardness until it breaks when bent. Next, the dried turmeric slices are made into powder form. by pounding with a mortar or with the help of a pestle blender or chopper blender. 2. A certain amount of turmeric powder 40 grams or adjust with the size of the Soxhlet apparatus, tightly wrapped like a shape lead using filter paper, then put it in Soxhlet apparatus set. Ethanol solvent 968 is introduced through cooling end as much as 1 & circulation (in this experiment 250 mL). Extraction was carried out at a temperature of 75-85 “C, soxhletation stopped when the liquid coming down from the cooler has no longer colored. The solvent of this ethanol extract is then evaporated using a tool. rotary vacuum evaporator or regular evaporator above water bath at a temperature of 40-50 ”C until it forms thick extract that is dark brown in color with a larger volume less than 50 mL. Ethanol extract of turmeric powder still contains compounds others that are non-polar such as oil and so on. To separate curcuminoids from other compounds nonpolar in nature, liquid-liquid extraction is carried out with n-hexane solvent using a separating funnel in the following way as follows. The thick extract obtained is put into separating funnel and added 1:1 n-hexane solvent (50 mL). This mixture is then shaken vigorously, after that let it sit for a while until it separates into two layers namely the ethanol phase and the n-hexane phase. The n-hexane phase is present in the upper layer, this phase contains components dissolve n-hexane, this phase is discarded. Next, in the next phase ethanol is added again with the same amount of n-hexane solvent, re-extraction is carried out. Extraction is carried out until clear h-hexane layer, which indicates that the ethanol phase has free from n-hexane soluble components. At this stage you can see the curcumin solid directly formed in the ethanol phase because the extract is quite concentrated so that saturation occurs. This ethanol phase is then put into a porcelain cup. and evaporate the solvent (ethanol) over a water bath at temperature 40-50”C. If the ethanol has evaporated, you will get curcuminoid powder that is yellow-orange in color. This powder then characterized using layer chromatography thin film (TLC), melting point, UV-Vis spectrum, and spectrum FTIR. Table 1 shows the results of the thin layer chromatography test. in the form of a retardation factor (RE) value, namely the comparison of the distance the distance traveled by the stain with the distance traveled by the eluent. In the table It can be seen that the Rf value between the extracted curcuminoids and standard curcumin, indicating the curcuminoid component consists of three compounds, namely curcumin, desmethoxycurcumin, and bisdesmethoxycurcumin. Table 1. Thin layer chromatography test results of Kieselgel 60F 254 0.2 mm thick Rf Curcumin Eluent Curcumin Compound name standard results" extraction Benzene:chlorothorm: 0.62 0.62 Curcumin ethanol 0.53 0.53 Desmethoxycurcumin 45:45:10 0.16 0.16 Bisdesmethoxycurcumin Benzene:chlorothorm: 0.58 0.58 Curcumin ethanol 0.45 0.45 Desmethoxycurcumin 5:4:1 0.34 0.34 Bisdesmethoxycurcumin Benzene:chlorothorm: 0.74 0.74 Curcumin ethanol 0.70 0.70 Desmethoxycurcumin 4:4:2 0, 67 0, 67 Bisdesmethoxycurcumin “BDH England Table 2 shows the results of the melting point test. shows that between the curcuminoids extracted and standard curcumin is the same substance. The presence of a small amount the difference is likely due to the humidity influencing to the melting point. Based on the melting point data between starts to melt and melts completely at less than £2”C indicates that the curcuminoid compounds extracted are sufficient pure Table 2. Melting point test using Stuart Melting Points Apparatus Compound name Melting point “C Starting to melt Melting completely Curcuminoid extraction results 174.0 176.0 Standard curcumin 173.9 175.6 Table 3 shows the spectrum data of the curcumin extracted and 5 standard curcumins that provide similar wavelengths with a difference of no more than 2 nm that can be tolerated. The wavelengths in the visible region are due to by the 7Tb7' electronic transition. 10 Table 3. UV-Vis spectrum data of standard curcumin and curcumin extraction results using dimethyl solvent sulfoxide (DMSO) Maximum wavelength (nm) Standard curcumin Curcumin extracted from extract 126 1425 447 449 Table 4 FTIR data of standard curcumin and curcumin products 15 extractions . - | Wavenumber (cm!) UguS TungSA Theoretical Curcumin Curcumin results extraction standards OH 3550-3200 3507.80 3347.819 C—0 1830-1530 1626.22 1625.698 1601.53 1590.985 C—Cc 1600-1430 1506, 69 1505,169 (aliphatic) C—Cc 1630-1400 1455.86 1407.781 (aromatic) C-0 phenol 1260-1000 1203, 93 1157,080 Table 4 shows the FTIR data of the extracted curcumin and standard curcumin has the same functional groups and is suitable theoretically. Another object of the present invention is to obtain an extract curcumin in powder form in a simple, easy way, fast and cheap with a fairly high yield, namely more of 28 of the dry weight of turmeric powder. Curcuminoid powder The results obtained can later be used as ingredients in direct drug manufacture or other purposes such as for the synthesis of complex compounds with metal ions, the manufacture of nanocurcuminoids for the same purpose.

Claims

1. Process of making curcuminoid extract from turmeric rhizome (Curcuma longa) with the following steps a. 40 grams of turmeric rhizome powder was extracted by soxhletation using 250 ml of ethanol 968 at a temperature of 75-85” Cj b. The results of the extraction stage a are evaporated using rotary vacuum evaporator or evaporated over a water bath at a temperature of 40-50”C until a thick extract of 50 is formed mL: Cc. The resulting thick extract stage b was carried out liquid-liquid extraction using n-hexane solvent with The 1:1 ratio is repeated until the n-hexane phase is reached. colorless three times: d. The extract produced in stage c. which contains curcuminoids in ethanol are evaporated with a water bath at a temperature of 40- 509C until a yellow-orange powder is obtained yield of more than 0.4% of the weight of wet turmeric or more of 28 weight of dry turmeric powder.

2. The process of making curcuminoid extract from turmeric rhizomes (Curcuma longa) according to claim 1, wherein in year c is carried out further shaking using a separating funnel with combination of ethanol 968 and n-hexane solvents with a ratio of 1:1,

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