Ternary deep eutectic solvent and method for extracting carthamin yellow and haematochrome through one-step method

Abstract

The invention discloses a ternary deep eutectic solvent and method for extracting carthamin yellow and haematochrome through a one-step method, and belongs to the technical field of traditional Chinese medicine extraction. The ternary deep eutectic solvent is a clear and transparent liquid prepared by mixing choline chloride, ethylene glycol and acetamide according to a molar ratio of 1: 3: 1 and heating. According to the method for extracting the carthamin yellow and the haematochrome by the one-step method, the ternary deep eutectic solvent is used as an extraction solution, and the synchronous extraction of the carthamin yellow and the haematochrome in the safflower is realized by adopting an ultrasonic extraction method. The ternary deep eutectic solvent disclosed by the invention is biodegradable, safe and environment-friendly, and pollution of a traditional organic solvent to the environment can be avoided. According to the method for extracting the safflower pigment through the ternary deep eutectic solvent one-step method, the mass transfer process can be enhanced, synchronous extraction of the safflower pigment is achieved, the resource utilization rate is increased, the extraction time is short, the extraction efficiency is high, energy consumption is low, long-time storage can be achieved, and important significance is provided for full utilization of pigment in the safflower traditional Chinese medicinal material.

Description

Technical Field

[0001] The invention relates to the technical field of extraction of effective components of traditional Chinese medicine, in particular to a ternary deep eutectic solvent and a method for extracting safflower yellow pigment and red pigment in one step. Background Art

[0002] Safflower is the dried tubular flower of Carthamus tinctorius L., a plant in the Asteraceae family. It is pungent and warm in nature, entering the Heart and Liver meridians. It promotes blood circulation, relieves menstruation, dissipates blood stasis, and relieves pain. It is clinically used to treat amenorrhea, dysmenorrhea, abdominal masses, chest pain, abdominal pain caused by blood stasis, and injuries from falls. It is a commonly used traditional Chinese medicine for promoting blood circulation and removing blood stasis. Safflower also contains important natural pigments, such as safflower yellows (hydroxysafflower yellow A and anhydrosafflower yellow B) and red pigment (safflower glycosides).

[0003] Currently, organic solvent extraction is the most common method for extracting the yellow and red pigments from safflower. However, this method suffers from cumbersome and complex procedures, as well as the inability to extract both the yellow and red pigments simultaneously due to their different properties. Furthermore, organic solvent extraction requires the use of large amounts of chemical solvents, which increases costs and creates an environmental burden during the subsequent solvent separation and recovery process.

[0004] On this basis, this application conducts in-depth research on the extraction process of yellow pigment and red pigment in safflower, and creates a new ternary deep eutectic solvent and method that can extract safflower yellow pigment and red pigment in one step, realizing the one-step efficient extraction of safflower yellow pigment and red pigment in safflower, providing important practical significance for the extraction and utilization of the effective ingredients of safflower Chinese medicinal materials. Summary of the Invention

[0005] The technical problem to be solved by the present invention is to provide a ternary deep eutectic solvent for extracting safflower yellow pigment and red pigment in one step, so that it can achieve a one-step efficient extraction of safflower yellow pigment and red pigment in safflower, and the natural deep eutectic solvent is biodegradable and environmentally friendly, thereby overcoming the shortcomings of the existing safflower pigment extraction method.

[0006] To solve the above technical problems, the present invention provides a ternary deep eutectic solvent for extracting safflower yellow pigment and red pigment in one step. The ternary deep eutectic solvent is a clear and transparent liquid formed by mixing choline chloride, ethylene glycol, and acetamide in a molar ratio of 1:3:1 and heating.

[0007] Further improvement, the preparation method of the ternary deep eutectic solvent is: take choline chloride, ethylene glycol, and acetamide in a molar ratio of 1:3:1, and heat and stir in a constant temperature water bath at 80° C. for 2 hours to obtain the obtained solvent.

[0008] As another improvement of the present invention, the present invention also provides a one-step method for extracting safflower yellow pigment and red pigment, which enables the efficient and synchronous extraction of safflower yellow pigment and red pigment. The method is simple, has a high extraction rate, low energy consumption, and is environmentally friendly, and can provide important practical significance for the extraction and utilization of the effective ingredients of safflower Chinese medicinal materials.

[0009] The extraction method of the present invention uses the ternary deep eutectic solvent for extracting safflower yellow pigment and red pigment in the one-step method as the extraction solution, and adopts ultrasonic extraction to achieve the simultaneous extraction of safflower yellow pigment and red pigment in safflower.

[0010] Specifically, the method includes the following steps:

[0011] (1) adding a certain amount of water to the ternary deep eutectic solvent and mixing uniformly to obtain an extraction solution, wherein the water content of the extraction solution is 10-20%;

[0012] (2) Take safflower powder, add the above extraction solution at a material-liquid ratio of 50-75 mg / mL, perform ultrasonic extraction, the ultrasonic temperature is 40-60℃, the ultrasonic time is 10-30 min, centrifuge, remove the supernatant, and obtain safflower yellow pigment and red pigment extract.

[0013] Further improvement: the water content of the extraction solution in step (1) is 12.8%; in step (2), the extraction solution is added at a material-liquid ratio of 50.5 mg / mL, and the ultrasonic temperature is 48°C and the ultrasonic time is 21 min.

[0014] In step (2), the ultrasonic power is 100 W and the ultrasonic frequency is 40 kHz.

[0015] The safflower yellow pigment and red pigment extract obtained in step (2) can achieve a degradation rate of less than 50% of the safflower yellow pigment and red pigment when stored in the dark at 0-25°C for 10 days.

[0016] As a further improvement, the safflower yellow pigment and red pigment extract obtained in step (2) can be stored at 4°C in the dark for 8 days, and the degradation rate of safflower yellow pigment and red pigment can be less than 30%.

[0017] After adopting such a design, the present invention has at least the following advantages:

[0018] 1. The ternary deep eutectic solvent for extracting safflower yellow pigment and red pigment in one step of the present invention is biodegradable, safe and environmentally friendly, and can avoid the pollution of traditional organic solvents to the environment.

[0019] 2. The one-step method for extracting safflower yellow pigment and red pigment of the present invention uses a natural ternary deep eutectic solvent as the extraction solution and adopts ultrasound-assisted extraction, which can enhance the mass transfer process, realize the simultaneous extraction of safflower yellow pigment and red pigment, improve resource utilization, and greatly shorten the extraction time, improve the extraction efficiency, and reduce energy consumption, which is conducive to maximizing the utilization of safflower resources. It can also greatly increase the shelf life of the extract, provide more favorable convenience for the actual use of the extract, and enhance the application prospects of pigments in more fields. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] The above is only an overview of the technical solution of the present invention. In order to more clearly understand the technical means of the present invention, the present invention is further described in detail below in conjunction with the accompanying drawings and specific embodiments.

[0021] Figure 1 This is a liquid phase detection chromatogram for detecting safflower yellow pigment and red pigment in the experiment of the present invention;

[0022] Figure 2 This is the pigment extraction rate result of the first round of solvent screening experiment of natural deep eutectic solvent in the experiment of the present invention;

[0023] Figure 3 This is the pigment extraction rate result of the second round of solvent screening experiment of natural deep eutectic solvent in the experiment of the present invention;

[0024] Figure 4 The pigment extraction rate results obtained by the single factor investigation experiment of each factor variable in the extraction process of the present invention, wherein (A) is the solid-liquid ratio factor, (B) is the extraction temperature factor, (C) is the extraction time factor, and (D) is the moisture content factor;

[0025] Figure 5 Schematic diagram of the response surface obtained by investigating various factors in the response surface optimization experiment of the extraction process of the present invention, including (A) solid-liquid ratio and extraction temperature, (B) solid-liquid ratio and extraction time, (C) solid-liquid ratio and moisture content, (D) extraction time and extraction temperature, (E) moisture content and extraction time, and (F) extraction temperature and moisture content;

[0026] Figure 6 The results of the stability test of different pigments by different extracts in the extraction process of the present invention are as follows: (A) HSYA, (B) AHSYB, and (C) Carthamin.

[0027] Figure 7 Fourier transform infrared spectra of the natural ternary deep eutectic solvent prepared by the present invention and the original solvent, wherein (a) is choline chloride, (b) is ethylene glycol, (c) is acetamide, and (d) is the natural ternary deep eutectic solvent;

[0028] Figure 8The Fourier transform infrared spectra of the safflower extract and safflower pigments obtained by the present invention, wherein (a) is the safflower extract obtained by NATDES extraction, (b) is HSYA, (c) is AHSYB, and (d) is Carthamin;

[0029] Figure 9 The following are scanning electron microscope images of safflower after extraction with various solvents in the present invention, wherein (a) is the original safflower, (b) is the safflower after ultrasonic-assisted methanol extraction, (c) is the safflower after ultrasonic-assisted water extraction, (d) is the safflower after ultrasonic-assisted choline chloride: ethylene glycol: lactic acid 1:3 extraction, (e) is the safflower after ultrasonic-assisted choline chloride: ethylene glycol 1:3 extraction, and (f) is the safflower after ultrasonic-assisted choline chloride: ethylene glycol: acetamide 1:3:1 extraction. DETAILED DESCRIPTION

[0030] Exemplary embodiments of the present invention will be described in more detail below with reference to the accompanying drawings. Although exemplary embodiments of the present invention are shown in the accompanying drawings, it should be understood that the present invention can be implemented in various forms and should not be limited by the embodiments set forth herein. Rather, these embodiments are provided to enable a more thorough understanding of the present invention and to fully convey the scope of the present invention to those skilled in the art.

[0031] It should be noted that if specific experimental steps or conditions are not specified in this example, the conventional experimental steps or conditions described in the literature in this field can be followed. The reagents or instruments used without indicating the manufacturer are all conventional reagents that can be purchased commercially.

[0032] Example 1

[0033] The one-step method for extracting safflower yellow pigment and red pigment from safflower comprises the following steps:

[0034] (1) Screening and preparation of extraction solvents:

[0035] The hydrogen acceptor (HBA) and hydrogen donor (HBD) listed in Table 1 below were mixed in the molar ratios listed and stirred at 80°C for 2 hours to obtain homogeneous, transparent deep eutectic solvents. Separately, extractions of safflower (Carthamus tinctorius) were performed using conventional deep eutectic solvents (L-proline:acetamide:water in a molar ratio of 1:1:2), choline chloride:glucose:water in a molar ratio of 5:2:5, and water and methanol as extraction solvents.

[0036] Table 1 Combination ratios of various extraction solvents

[0037]

[0038] (2) Extraction method:

[0039] Approximately 100 mg of safflower freeze-dried powder was weighed and added to 2 mL of the above-prepared extraction solvent. The mixture was vortexed for 5 minutes and then subjected to ultrasonic extraction at 50°C and 40 kHz for 20 minutes at 100 W. After extraction, the mixture was centrifuged at 13,000 rpm for 10 minutes to remove the residue. This yielded the extracts prepared in the different extraction solvents.

[0040] (3) Content determination:

[0041] Take each extract obtained in (2) above and detect safflower yellow pigment and red pigment respectively. Among them, safflower yellow pigment uses hydroxysafflower yellow A (HSYA) and anhydrosafflower yellow B (AHSYB) as detection indicators, and red pigment uses carthamin as detection indicator. The specific detection method is as follows:

[0042] Yellow pigment: Waters SunFire C 18 The chromatographic column was 4.6 mm × 150 mm, 5 μm. The mobile phase was methanol (A)-0.7% phosphoric acid (B) with gradient elution (0-10 min, 10-42% A; 10-15 min, 42-45% A; 15-20 min, 45-60% A; 20-22 min, 60-90% A; 22-23 min, 90-10% A; 23-24 min, 10% A; flow rate 1.0 mL min -1 : Detection wavelength 403 nm; column temperature 25°C, injection volume 10 μL. Figure 1 (A) and (B) show the chromatograms of HSYA and AHSYB standards and safflower extract obtained under the HPLC conditions, respectively.

[0043] Safflower glycosides: Waters ultra-high performance liquid chromatography, SunFire C 18 Chromatographic column (4.6 mm × 250 mm, 5 μm). The mobile phase consisted of methanol (A), 0.3% phosphoric acid in water (B), and acetonitrile (C), with an equal volume elution ratio of 5:57:38 (v / v / v). The detection wavelength was maintained at 520 nm, the column temperature was maintained at 35°C, and the flow rate was 1.0 mL min. −1 The injection volume was 10 μL. Figure 1 (C) and (D) show the chromatograms of safflower glycoside standard and safflower extract obtained under the HPLC conditions, respectively.

[0044] (4) Results analysis

[0045] The results of the determination of the content of different pigments in each extract are shown in Table 2 and Attached. Figure 2 shown.

[0046] Table 2 Results of determination of the content of different pigments in the above extracts (mg / g)

[0047]

[0048] From Table 2 above and the attached Figure 2 As shown in the figure, when the extraction solvent is BE:EG 1:2, ChCl:EG 1:3, and ChCl:LA 1:1, both safflower yellow pigment and red pigment can be extracted, among which ChCl:EG 1:3 is the best.

[0049] Example 2

[0050] Based on the extraction solvent with a molar ratio of choline chloride to ethylene glycol of 1:3 obtained in Example 1 above, further extraction solvent screening was performed.

[0051] The hydrogen acceptor (HBA) and hydrogen donor (HBD) were mixed in the molar ratios shown in Table 3 below and stirred at 80°C for 2 h to obtain a uniform and transparent deep eutectic solvent. The extraction method of Example 1 was used again to extract the Chinese medicinal material safflower, and the yellow pigment and red pigment contents of each extract were determined according to the content determination method of Example 1. The results are shown in Table 4 and the attached Figure 3 shown.

[0052] Table 3 Combination ratios of various extraction solvents

[0053]

[0054] Table 4 Results of determination of the content of different pigments in the above extracts (mg / g)

[0055]

[0056] From Table 4 above and the attached Figure 3 As shown in the figure, when the extraction solvent is ChCl:EG:AM 1:3:1, it can better take into account the extraction of safflower yellow pigment and red pigment. Compared with the results of ChCl:EG 1:3 in Table 2, the natural ternary deep eutectic solvent formed by choline chloride, ethylene glycol and acetamide can more effectively extract safflower yellow pigment and red pigment simultaneously.

[0057] Example 3 Single factor experiment

[0058] The natural ternary deep eutectic solvent of ChCl:EG:AM 1:3:1 selected in Example 2 was selected as the safflower extraction solvent, and a single-factor experiment on the material-liquid ratio, extraction temperature, extraction time, and water content was conducted on the extraction method.

[0059] (1) Single factor experiment of material-liquid ratio:

[0060] 300 mg of safflower freeze-dried powder was weighed and added to 2, 3, 4, 6, and 12 mL of a natural ternary deep eutectic solvent, respectively. The mixture was vortexed for 5 minutes and then extracted at 50°C and 40 kHz in an ultrasonic device with a power of 100 W for 20 minutes. After extraction, the mixture was centrifuged at 13,000 rpm for 10 minutes to remove the residue. This yielded extracts with different solid-liquid ratios.

[0061] (2) Extraction temperature single factor experiment:

[0062] 200 mg of safflower freeze-dried powder was weighed and added to 2 mL of a natural ternary deep eutectic solvent. The mixture was vortexed for 5 minutes and then extracted in an ultrasonic device with a power of 100 W for 20 minutes at 20, 30, 40, 50, and 60°C (40 kHz). After extraction, the mixture was centrifuged at 13,000 rpm for 10 minutes to remove the residue. This yielded extracts prepared at different extraction temperatures.

[0063] (3) Single factor experiment of extraction time:

[0064] 200 mg of safflower freeze-dried powder was weighed and added to 2 mL of a natural ternary deep eutectic solvent. The mixture was vortexed for 5 minutes and then extracted in an ultrasonic device with a power of 100 W at 50°C and a frequency of 40 kHz for 10, 20, 30, 40, and 50 minutes, respectively. After extraction, the mixture was centrifuged at 13,000 rpm for 10 minutes to remove the residue. This yielded the extracts obtained at different extraction times.

[0065] (4) Single factor experiment on moisture content:

[0066] Different amounts of water were added to the natural ternary deep eutectic solvent of ChCl:EG:AM 1:3:1, so that the volume proportion of water in the extraction solvent was 0, 10, 20, 30, and 40%, respectively.

[0067] Weigh 200 mg of freeze-dried safflower powder and add it to 2 mL of the extraction solvents described above with varying moisture contents. Vortex the mixture for 5 minutes and then extract it in an ultrasonic device with a power of 100 W at 50°C and a frequency of 40 kHz for 30 minutes. After extraction, centrifuge the mixture at 13,000 rpm for 10 minutes to remove the residue, thereby obtaining extracts with varying moisture contents.

[0068] The extracts obtained from the above single factor experiments were subjected to the determination of yellow pigment and red pigment content according to the content determination method of Example 1. The results are shown in the attached Figure 4 shown.

[0069] From the attached Figure 4 As can be seen from the results, the effects of each single factor on the extraction rate of safflower yellow pigment were not very obvious, but the extraction rate of safflower glycosides was significantly affected. The results showed that the extraction efficiency of safflower yellow pigment and red pigment was high when the solid-liquid ratio was 50-75 mg / mL, the extraction temperature was 40-60℃, the extraction time was 10-30 min, and the moisture content was 10-20%. The optimal conditions were: solid-liquid ratio of 50 mg / mL, extraction temperature of 50℃, extraction time of 20 min, and moisture content of 10%.

[0070] Example 4 Response Surface Optimization

[0071] The water content, extraction time, material-liquid ratio, and extraction temperature of the natural ternary deep eutectic solvent obtained in Example 3 were initially selected as the investigation factors, and the safflower glycoside extraction rate was used as the evaluation index. 46 response surface test points were designed using 4 factors and 3 levels to determine the optimal process conditions. Each experimental point was repeated three times and the average value was taken. The results are shown in the attached figure. Figure 5 shown.

[0072] According to the experimental results, Design Expert 10.0 was used to fit the test results and obtain the mathematical regression model equation of safflower glycoside extraction rate (Y) and solid-liquid ratio (A), temperature (B), time (C), and moisture content (D):

[0073] Y=2.12-0.0983A-0.1842B+0.0883C+0.3325D-0.2800AB+0.1500AC+0.0950AD-0.1100BC-0.1775BD+0.05CD-0.1899A²-0.6687B²-0.3874C²-0.6562D², perform a significance test on the model.

[0074] From the attached Figure 5 The effects of individual variables and their interactions on the extraction rate of safflower glycosides were investigated. The three-dimensional response surface plots for AC, AD, BC, and CD were relatively flat, indicating no significant interaction between the two variables (p > 0.05). However, the three-dimensional response surface plots for AB and BD were steep, indicating a significant interaction between the two variables (p < 0.05), consistent with the results of the analysis of variance. Ultimately, based on practical feasibility, the optimal extraction process conditions were revised to: a solid-liquid ratio of 50.5 mg / mL, an extraction temperature of 48°C, an extraction time of 21 min, and a water content of 12.8%.

[0075] In this example, three sets of verification experiments were conducted in parallel according to the optimal optimization process. The average yield of safflower glycosides was 2.1562 mg / g, which was basically consistent with the predicted value of 2.19584 mg / g, and the RSD value was 2.83% (< 3.0%), indicating that the established model is accurate and feasible, the optimized process is stable and feasible, and the safflower glycoside extraction rate can be above 95%.

[0076] Furthermore, in three parallel validation experiments conducted using the optimized process for safflower glycosides, the mean yields of hydroxysafflower yellow A and anhydrosafflower yellow B were 11.5838 mg / g and 6.6975 mg / g, respectively. These yields were within an acceptable range of 13% of the actual yields. Therefore, the optimal extraction process established in this example is suitable for the simultaneous extraction of safflower glycosides, hydroxysafflower yellow A, and anhydrosafflower yellow B.

[0077] Example 5 Extraction stability test

[0078] The safflower medicinal material was extracted using the extraction process conditions finally determined in Example 4 to obtain safflower extract 1. The safflower medicinal material was then extracted using methanol and water as extraction solvents to obtain safflower extracts 2 and 3, respectively.

[0079] HSYA, AHSYB, and Carthamin in extracts 1, 2, and 3 were tested and recorded as the original test values. Extracts 1, 2, and 3 were then placed in three different environments (4°C in the dark, 25°C in the dark, and 25°C alternating day and night) and tested every two days to monitor the changes in the concentrations of the three pigments over time. The results are shown in the attached Figure 6 shown.

[0080] Figure 6 The stability test results of different extracts on different pigments are shown, including (A) HSYA, (B) AHSYB, and (C) Carthamin. Figure 6 It can be seen that 4°C in the dark and 25°C in the dark have better preservation advantages for HSYA, AHSYB, and carthamin than 25°C in the day-night cycle, with carthamin being particularly advantageous. For example, the degradation rate of safflower glycosides at 25°C in the day-night cycle was greater than 80% after 10 days of storage. However, the degradation rate was less than 50% after 10 days of storage at 4°C in the dark and 25°C in the dark, with 4°C in the dark achieving the best results. These results indicate that storage conditions are crucial for maintaining the stability of the beneficial nutrients of safflower pigments after extraction.

[0081] It was also found that the stability of each pigment in different extracts varied significantly over time. For example, HSYA and AHSYB exhibited greater stability among the three pigments, and their degradation rates were not significantly affected by the different extracts. In contrast, safflower glycoside degraded more rapidly, especially in aqueous extracts. Even when stored at 4°C in the dark, it was essentially undetectable after four days. However, storage in the natural ternary deep eutectic solvent choline chloride-ethylene glycol-acetamide (ChCl-EG-AM) significantly improved safflower glycoside's stability. For example, after eight days of storage at 4°C in the dark, the preservation rate of safflower glycoside remained greater than 70%. These results demonstrate that the natural ternary deep eutectic solvent ChCl-EG-AM not only enables the one-step extraction of safflower pigment components but also serves as a storage medium for safflower pigments, extending the shelf life of the extract.

[0082] Example 6 Related Characterization

[0083] (1) Infrared spectroscopy

[0084] The potassium bromide tablet method was used: a certain amount of HSYA monomer, Carthamin monomer, AHSYB monomer, choline chloride, and acetamide samples were mixed with dry potassium bromide powder, ground, and pressed into thin sheets for FT-IR analysis of solid samples.

[0085] Take appropriate amounts of ethylene glycol, natural ternary deep eutectic solvent, and safflower extract of natural ternary deep eutectic solvent, respectively, and drop them on potassium bromide tablets to complete the preparation of liquid samples.

[0086] The above sample was prepared at room temperature and 400-4000 cm -1 Infrared spectrum scanning was performed within the range. The results are shown in the attached Figure 7 and 8 shown.

[0087] Figure 7 The Fourier transform infrared spectra of the natural ternary deep eutectic solvent and the original solvent, where (a) is choline chloride, (b) is ethylene glycol, (c) is acetamide, and (d) is the natural ternary deep eutectic solvent. Figure 7 It can be seen that compared with a, b, and c, the spectrum of the natural ternary deep eutectic solvent in d is 1500 cm -1 The sharp peak at 1700 cm indicates that the carbonyl group and the amino group in the original solvent have undergone Schiff base condensation reaction. -1 The carbonyl absorption peak at 3300 cm-1 is weakened or even disappears, which also proves the occurrence of condensation reaction. -1 The hydroxyl group at the position shows an obvious blue shift, indicating the formation of intermolecular hydrogen bonds.

[0088] Figure 8The following are Fourier transform infrared spectra of safflower extract and safflower pigments extracted using natural ternary deep eutectic solvents, where (a) is safflower extract extracted using NATDES, (b) is HSYA, (c) is AHSYB and (d) is Carthamin. Figure 8 It can be seen that the infrared absorption peaks of bcd monomers appear in the safflower extract, indicating that the natural ternary deep eutectic solvent has a good extraction effect on safflower yellow pigment and red pigment. It is worth noting that compared with the monomer, the safflower extract has a strong absorption peak at 3300 cm -1 The hydroxyl absorption peak of the hydroxyl group was blue-shifted to 1700 cm -1 The C=O absorption peak of the solvent is red-shifted compared to the bcd peak and blue-shifted compared to the solvent, indicating that the natural ternary deep eutectic solvent forms intermolecular hydrogen bonds with the safflower yellow and red pigments, resulting in good interaction. This example also demonstrates that the natural ternary deep eutectic solvent can effectively extract the safflower yellow and red pigment components.

[0089] (2) SEM electron microscope

[0090] The safflower medicinal material was extracted according to the extraction method in Example 1 using choline chloride: ethylene glycol: lactic acid 1:3:1, choline chloride: ethylene glycol 1:3, choline chloride: ethylene glycol: acetamide 1:3:1, methanol, and water as extraction solvents. After extraction, the safflower residue was filtered and naturally air-dried to obtain dried residue products after extraction with each extraction solvent.

[0091] Then, the dried medicinal residues after extraction with each extraction solvent and the original medicinal material of safflower were placed on the stage, coated with gold palladium, and the morphology of each sample was analyzed under a scanning electron microscope. Figure 9 shown.

[0092] Figure 9 The scanning electron microscope images of safflower after extraction with various solvents are shown, where (a) is the original safflower, (b) is the safflower after ultrasonic-assisted methanol extraction, (c) is the safflower after ultrasonic-assisted water extraction, (d) is the safflower after ultrasonic-assisted choline chloride: ethylene glycol: lactic acid 1:3 extraction, (e) is the safflower after ultrasonic-assisted choline chloride: ethylene glycol 1:3 extraction, and (f) is the safflower after ultrasonic-assisted choline chloride: ethylene glycol: acetamide 1:3:1 extraction. Figure 8It can be seen that the surface structure of the original safflower medicinal material is complete and smooth. After ultrasonic-assisted methanol and water extraction, the structure of the safflower medicinal material is relatively complete, and fine cracks appear on the surface. After ultrasonic-assisted natural ternary deep eutectic solvent extraction, the surface structure of the safflower medicinal material showed varying degrees of damage, pores appeared, and the internal structure was exposed. Among them, the damage to the choline chloride: ethylene glycol: acetamide 1:3:1 group was the most significant. This also shows that the natural ternary deep eutectic solvent choline chloride: ethylene glycol: acetamide 1:3:1 has a strong extraction effect on the pigments in safflower.

[0093] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any form. Those skilled in the art can make some simple modifications, equivalent changes or modifications based on the technical content disclosed above, which all fall within the scope of protection of the present invention.

Claims

1. A ternary deep eutectic solvent for extracting safflower yellow pigment and red pigment in one step, characterized in that: The ternary deep eutectic solvent is a clear and transparent liquid formed by mixing choline chloride, ethylene glycol, and acetamide in a molar ratio of 1:3:1 and heating.

2. The ternary deep eutectic solvent for extracting safflower yellow pigment and red pigment in one step according to claim 1, characterized in that: The preparation method of the ternary deep eutectic solvent is as follows: choline chloride, ethylene glycol, and acetamide are mixed in a molar ratio of 1:3:1, and heated and stirred in a constant temperature water bath at 80° C. for 2 h to obtain the obtained solvent.

3. A one-step method for extracting safflower yellow pigment and red pigment, characterized in that: The ternary deep eutectic solvent for extracting safflower yellow pigment and red pigment in one step according to claim 1 or 2 is used as the extraction solution, and ultrasonic extraction is used to achieve the simultaneous extraction of safflower yellow pigment and red pigment in safflower.

4. The method for extracting safflower yellow and red pigment by one-step method according to claim 3, wherein The method comprises the following steps: (1) adding a certain amount of water to the ternary deep eutectic solvent and mixing uniformly to obtain an extraction solution, wherein the water content of the extraction solution is 10-20%; (2) Take safflower powder, add the above extraction solution at a material-liquid ratio of 50-75 mg / mL, perform ultrasonic extraction, the ultrasonic temperature is 40-60℃, the ultrasonic time is 10-30 min, centrifuge, remove the supernatant, and obtain safflower yellow pigment and red pigment extract.

5. The method for extracting safflower yellow and red pigment by one-step method according to claim 4, wherein The water content of the extraction solution in step (1) is 12.8%; in step (2), the extraction solution is added at a material-liquid ratio of 50.5 mg / mL, and the ultrasonic temperature is 48° C. and the ultrasonic time is 21 min.

6. The method for extracting safflower yellow and red pigment by one-step method according to claim 5, characterized in that, In step (2), the ultrasonic power is 100 W and the ultrasonic frequency is 40 kHz.

7. The method for extracting safflower yellow and red pigment by one-step method according to claim 4, wherein The safflower yellow pigment and red pigment extract obtained in step (2) can achieve a degradation rate of less than 50% of the safflower yellow pigment and red pigment when stored in the dark at 0-25°C for 10 days.

8. The method for extracting safflower yellow and red pigment by one-step method according to claim 7, wherein The safflower yellow pigment and red pigment extract obtained in step (2) can achieve a degradation rate of less than 30% of the safflower yellow pigment and red pigment when stored at 4° C. in the dark for 8 days.

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