Preparation method of low-odor arnebia euchroma (juss.) johnst. Extract and product and application thereof

Abstract

This invention belongs to the field of cosmetic raw material preparation technology, specifically relating to a method for preparing a low-odor Xinjiang Lithospermum extract, its product, and its application. The method includes: raw material pretreatment: drying and pulverizing Xinjiang Lithospermum raw material to obtain pretreated material; first-stage extraction: loading the pretreated material into a supercritical fluid extraction device, adding a composite entrainer for extraction, and collecting the first fraction in a first separator; second-stage extraction: collecting a second fraction rich in naphthoquinone components in a second separator; and post-treatment: concentrating the second fraction and removing the alcohol solvent to obtain the low-odor Xinjiang Lithospermum extract. This invention can separate and discard most of the odor-causing volatile components in the raw material under mild conditions in the first stage, and then efficiently extract the core active substances of naphthoquinone in the second stage, achieving a significant reduction in the odor of the extract and a significant improvement in its sensory quality.

Description

Technical Field

[0001] This invention belongs to the field of cosmetic raw material preparation technology, specifically relating to a method for preparing a low-odor Xinjiang Lithospermum extract, its product, and its application. Background Technology

[0002] Xinjiang Lithospermum ( Arnebia euchroma As a traditional and precious Chinese medicinal herb, the naphthoquinone pigments (such as shikonin and acetylshikonin) abundant in its roots have been proven by studies to have multiple biological activities such as anti-inflammatory, antioxidant, wound healing promotion and anti-skin photoaging, showing great application potential in the field of high-end cosmetics and functional skin care products.

[0003] However, Xinjiang purple gromwell root raw materials and their conventional extracts typically possess a strong and persistent peculiar odor, primarily stemming from volatile small molecules and some unstable components. This odor not only severely impacts the sensory experience and consumer acceptance of the product but may also negatively affect formulation stability, becoming a bottleneck restricting its large-scale application in high-quality cosmetics. Traditional solvent extraction methods (such as ethanol extraction) or single supercritical carbon dioxide extraction processes often struggle to selectively remove or significantly reduce these unpleasant odor substances while efficiently enriching the active ingredient naphthoquinone, frequently facing the contradiction of balancing "efficacy enhancement" and "odor removal."

[0004] Currently, although some studies have attempted to deodorize extracts through post-processing techniques (such as adsorption and molecular distillation), these methods are typically cumbersome, result in high rates of active ingredient loss, and may introduce new impurities or degrade heat-sensitive components. Therefore, developing an integrated green preparation technology that can achieve efficient extraction of active ingredients and synergistic removal of unpleasant odors from the extraction source is crucial for enhancing the application value of Xinjiang Lithospermum in the cosmetics field. Summary of the Invention

[0005] The purpose of this section is to outline some aspects of the embodiments of the present invention and to briefly describe some preferred embodiments.

[0006] As one aspect of the present invention, the present invention provides a method for preparing a low-odor Xinjiang Lithospermum extract, which includes the following steps: (1) Raw material pretreatment: The raw material of Xinjiang purple gromwell is dried and crushed to obtain pretreated material; (2) First stage extraction: The pretreated material is loaded into a supercritical extraction device, a composite entrainer is added, extraction is carried out, and the first fraction is collected in the first separator; The composite entrainer comprises a lipid material and an alcohol solvent, wherein the lipid material is selected from at least one of glyceryl monostearate, glyceryl 1,3-distearate, and ethyl oleate; (3) Second stage extraction: After the first stage extraction is completed, the second fraction rich in naphthoquinones is collected in the second separator; (4) Post-processing: The second fraction is concentrated to remove the alcohol solvent, and the low-odor Xinjiang Lithospermum extract is obtained.

[0007] As a preferred embodiment of the preparation method described in this invention, in step (2), the alcohol solvent is an aqueous ethanol solution with a volume concentration of 95% or anhydrous ethanol; the extraction is carried out at an extraction pressure of 8-15 MPa and an extraction temperature of 40-50℃.

[0008] In a preferred embodiment of the preparation method described in this invention, the mass ratio of the lipid material to the alcohol solvent in the composite entrainer is 1:1-4.

[0009] As a preferred embodiment of the preparation method described in this invention, in step (2), the first stage extraction is carried out for 1-2 hours under a CO2 flow rate of 20-30 L / h.

[0010] As a preferred embodiment of the preparation method described in this invention, in step (2), the pressure of the first separator is 4-5 MPa and the temperature is 30-35 ℃.

[0011] As a preferred embodiment of the preparation method described in this invention, in step (3), the second stage of extraction involves adjusting the extraction pressure to 30-40 MPa and extracting for 2-3 hours at an extraction temperature of 40-50 ℃ and a CO2 flow rate of 40-50 L / h.

[0012] As a preferred embodiment of the preparation method described in this invention, in step (4), the concentration is carried out by rotary evaporation at 40-60°C.

[0013] As a preferred embodiment of the preparation method described in this invention, in step (1), the drying temperature is 40-60℃; the pulverization is pulverization to pass through a 20-40 mesh sieve.

[0014] The present invention also provides a method for preparing the low-odor Xinjiang Lithospermum extract, wherein the Xinjiang Lithospermum extract contains naphthoquinones as its active ingredients, including shikonin, isovaleroshikonin, acetylshikonin, deoxyshikonin, β-hydroxyisovaleroshikonin, β,β-dimethylacryloylacanine, isobutyryloylshikonin, and β-acetoxyisovaleroylacanine.

[0015] The present invention also provides the use of the Xinjiang Lithospermum extract in the preparation of cosmetics for anti-skin aging, anti-oxidation and / or anti-skin cell ferroptosis.

[0016] The beneficial effects of this invention are as follows: By employing a composite entrainer with a specific composition in conjunction with a two-stage supercritical CO2 extraction process, this invention creatively integrates the directional enrichment of the target active ingredient and the selective removal of volatile odor substances into a continuous preparation method. Under mild conditions, most of the odor-causing volatile components in the raw materials are separated and discarded in the first stage, and then naphthoquinone-like core active substances are efficiently extracted in the second stage, resulting in a significant reduction in the odor of the extract and a significant improvement in its sensory quality.

[0017] The extract prepared by this method not only retains the inherent high bioactivity of Xinjiang Lithospermum erythrorhizon, but also effectively preserves its anti-skin aging, anti-oxidative stress, and photoaging-related cell damage inhibitory effects. The entire process is green, efficient, and controllable, and the resulting product has uniform color, odor, and physicochemical properties, significantly broadening the application scope and compatibility of Xinjiang Lithospermum erythrorhizon extract in high-end cosmetic formulations. Attached Figure Description

[0018] To more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings used in the description of the embodiments will be briefly introduced below, wherein: Figure 1 The image shows the gas chromatography-mass spectrometry chromatogram of the low-odor Xinjiang Lithospermum extract obtained in Example 1.

[0019] Figure 2 The image shows the gas chromatography-mass spectrometry (GC-MS) chromatogram of the extract of Lithospermum erythrorhizon obtained in Comparative Example 3.

[0020] Figure 3 This is a staining image of β-galactosidase (β-gal) in test example 1.

[0021] Figure 4 The liquid chromatogram is shown for the low-odor Xinjiang Lithospermum extract obtained in Example 1.

[0022] Figure 5 The image shows the liquid chromatogram of the extract of Lithospermum erythrorhizon obtained in Comparative Example 3. Detailed Implementation

[0023] To make the above-mentioned objectives, features and advantages of the present invention more apparent and understandable, the specific embodiments of the present invention will be described in detail below with reference to specific examples.

[0024] Liquid chromatography detection method: A 5 µm Thermo Fisher C18 column (250 × 4.6 mm) was used. The mobile phase was: mobile phase A: acetonitrile, mobile phase B: 0.05% formic acid solution, isocratic elution, A:B (v / v) = 70:30, 0-30 min, detection wavelength: 516 nm, injection volume: 10 µL, time: 30 min, column temperature: 30 ℃. The retention times were as follows: shikonin: 5.33 min, β-hydroxyisovalerylshikonin: 6.616 min, acetylshikonin: 8.201 min, β-acetoxyisovalerylacanine: 11.884 min, deoxyshikonin: 13.126 min, isobutyrylshikonin: 14.724 min, β,β-dimethylacryloylacanine: 17.690 min, isovaerylshikonin: 19.322 min.

[0025] GC-MS Detection Method: The test solution was prepared with anhydrous ethanol at a total naphthoquinone concentration of 1%. GC-MS System: 8890A-5977C GC-MS system, Agilent Technologies, USA. Column: HP-5MS (30.0m × 250μm, 0.25μm); Initial temperature: 60℃, hold for 2 min; ramp up to 300℃ at 15℃ / min, hold for 5 min; Vaporization chamber temperature: 250℃; Transfer line temperature: 280℃; Carrier gas: He; Carrier gas flow rate: 1.0 mL / min; Splitless; Injection volume: 1 μL. Mass Spectrometry Conditions: EI source; Electron energy: 70 eV; Ion source temperature: 230℃; Quadrupole: 150℃; Scan mode: Scan; Scan mass range: 30–550 u; Solvent delay: 3 min. The detected components were qualitatively analyzed using the retention times of the MS databases NIST17 and NIST20; column bleed peaks were removed from the database screening results, and solvent absorption peaks were removed from the data processing results.

[0026] Supercritical fluid extraction equipment: Nantong Huaan Supercritical Fluorescence Extraction Co., Ltd., HA220-50-06-C. High-performance liquid chromatography: Agilent, model 1260 Infinity II. Glyceryl monostearate: CAS No. 123-94-4, Sinopharm Chemical Reagent Co., Ltd., item number 3009322911; 1,3-distearate: CAS No. 504-40-5, Shanghai Yuanye Biotechnology Co., Ltd., item number B74100; Ethyl oleate: CAS No. 111-62-6, Shanghai Maclean Biochemical Technology Co., Ltd., item number E787417; Anhydrous ethanol: CAS No. 64-17-5, Sinopharm Chemical Reagent Co., Ltd., item number 10009218.

[0027] Example 1: (1) Raw material pretreatment: Take Xinjiang purple gromwell (root) medicinal material dried at 50 ℃ and crush it through a 30 mesh sieve.

[0028] (2) Extraction: First stage of extraction: 1 kg of sieved material was loaded into a supercritical extraction vessel and an entrainer composed of 0.5 kg of glyceryl monostearate and 1.5 kg of 95 wt% ethanol aqueous solution was added. Extraction was carried out for 1 h at an extraction vessel pressure of 10 MPa, a temperature of 50 ℃, a CO2 flow rate of 25 L / h, a separation vessel I pressure of 6 MPa, a separation vessel I temperature of 35 ℃, a separation vessel II pressure of 4 MPa, and a separation vessel II temperature of 30 ℃. At this time, the liquid released from the separation vessel II was 105.4 g of Xinjiang Lithospermum extract with a strong odor. Second stage of extraction: The pressure of the supercritical extraction vessel was adjusted to 35 MPa, the temperature to 40 ℃, and the CO2 flow rate to 40 L / h for extraction for 2 h. At this time, the entrainer was transferred to the separation vessel I and the liquid in the separation vessel I was collected. The obtained liquid was concentrated in a rotary evaporator at 50 ℃ to remove ethanol and obtain Xinjiang Lithospermum extract with a low odor.

[0029] Detection: High-performance liquid chromatography (HPLC) was used to detect naphthoquinones from Xinjiang lithospermum. Eight components—shikonin, isovalerylshikonin, acetylshikonin, deoxyshikonin, β-hydroxyisovalerylshikonin, β,β-dimethylacryloylacanine, isobutyryloylshikonin, and β-acetoxyisovalerylacanine—were quantitatively analyzed. The total naphthoquinone yield from Xinjiang lithospermum was 4.2%, with a generally faint and indistinct odor. GC-MS results showed a significant decrease in the absorption peaks of volatile odor components (such as isovaleric acid, ethyl octanoate, ethyl decanoate, and ethyl palmitate).

[0030] Yield % = (M total naphthoquinone from Xinjiang Lithospermum / M raw material mass) × 100%.

[0031] In the formula: M, total naphthoquinones from Xinjiang Lithospermum, is the sum of the actual masses of the eight naphthoquinones from Xinjiang Lithospermum extract with low odor. M, raw material mass, is the dry weight of the Xinjiang Lithospermum raw material.

[0032] Example 2: (1) Raw material pretreatment: Take Xinjiang purple gromwell (root) medicinal material dried at 50 ℃ and crush it through a 30 mesh sieve.

[0033] (2) Extraction: First stage of extraction: 1 kg of sieved material was loaded into a supercritical extraction vessel and an entrainer composed of 0.8 kg of 1,3-distearate glyceryl ester and 2 kg of anhydrous ethanol was added. Extraction was carried out for 1 h at a pressure of 15 MPa, a temperature of 50 °C, a CO2 flow rate of 20 L / h, a pressure of 8 MPa in separation vessel I, a temperature of 35 °C in separation vessel I, a pressure of 5 MPa in separation vessel II, and a temperature of 30 °C in separation vessel II. At this time, the liquid released from separation vessel II was 130.2 g of Xinjiang Lithospermum extract with a strong odor. Second stage of extraction: The pressure of the supercritical extraction vessel was adjusted to 30 MPa, the temperature to 45 °C, and the CO2 flow rate to 45 L / h for 2.5 h. At this time, the entrainer was transferred to separation vessel I and the liquid in separation vessel I was collected. The obtained liquid was concentrated in a rotary evaporator at 50 °C to remove ethanol and obtain Xinjiang Lithospermum extract with a low odor.

[0034] Detection: High performance liquid chromatography (HPLC) was used to detect naphthoquinones from Xinjiang lithospermum. Quantitative analysis was performed on eight components: shikonin, isovaleryl shikonin, acetyl shikonin, deoxyshikonin, β-hydroxyisovaleryl shikonin, β,β-dimethylacryloyl argentin, isobutyryl shikonin, and β-acetoxyisovaleryl argentin. The actual yield of total naphthoquinones from Xinjiang lithospermum was 4.0%. The overall odor was faint and not obvious.

[0035] Example 3: (1) Raw material pretreatment: Take Xinjiang purple gromwell (root) medicinal material dried at 50℃ and crush it through a 30-mesh sieve.

[0036] (2) Extraction: First stage of extraction: 1 kg of sieved material was loaded into a supercritical extraction vessel and an entrainer composed of 1 kg of ethyl oleate and 1.5 kg of 95 wt% ethanol aqueous solution was added. Extraction was carried out for 1 h at an extraction vessel pressure of 12 MPa, a temperature of 50℃, a CO2 flow rate of 25 L / h, a separation vessel I pressure of 8 MPa, a separation vessel I temperature of 35 ℃, a separation vessel II pressure of 4 MPa, and a separation vessel II temperature of 30℃. At this time, the liquid released from the separation vessel II was 126.5 g of Xinjiang Lithospermum extract with a strong odor. Second stage of extraction: The pressure of the supercritical extraction vessel was adjusted to 40 MPa, the temperature to 45℃, and the CO2 flow rate to 50 L / h for 3 h. At this time, the entrainer was transferred to the separation vessel I and the liquid in the separation vessel I was collected. The obtained liquid was concentrated in a rotary evaporator at 50 ℃ to remove ethanol and obtain Xinjiang Lithospermum extract with a low odor.

[0037] Detection: High performance liquid chromatography (HPLC) was used to detect naphthoquinones from Xinjiang lithospermum. Quantitative analysis was performed on eight components: shikonin, isovaleryl shikonin, acetyl shikonin, deoxyshikonin, β-hydroxyisovaleryl shikonin, β,β-dimethylacryloyl argentin, isobutyryl shikonin, and β-acetoxyisovaleryl argentin. The measured total naphthoquinone yield from Xinjiang lithospermum was 3.9%. The overall odor was faint and not obvious.

[0038] Comparative Example 1: (1) Raw material pretreatment: Take Xinjiang purple gromwell (root) medicinal material dried at 50℃ and crush it through a 30-mesh sieve.

[0039] (2) Extraction: First stage of extraction: 1 kg of sieved material was loaded into a supercritical extraction vessel and extracted for 1.5 h at an extraction vessel pressure of 8 MPa, a temperature of 50 ℃, a CO2 flow rate of 30 L / h, a separation vessel I pressure of 7 MPa, a separation vessel I temperature of 35 ℃, a separation vessel II pressure of 4 MPa, and a separation vessel II temperature of 30 ℃. At this time, the liquid discharged from the separation vessel II was 5.5 g of Xinjiang Lithospermum extract. Second stage of extraction: The pressure of the supercritical extraction vessel was adjusted to 40 MPa, the temperature to 50 ℃, and the CO2 flow rate to 50 L / h for 3 h. The liquid in the separation vessel I was collected to obtain Xinjiang Lithospermum extract.

[0040] Detection: Total naphthoquinones from Xinjiang Lithospermum were determined by high performance liquid chromatography (HPLC). Eight components—shikonin, isovalerylshikonin, acetylshikonin, deoxyshikonin, β-hydroxyisovalerylshikonin, β,β-dimethylacryloylacanine, isobutyryloylshikonin, and β-acetoxyisovalerylacanine—were quantitatively analyzed. The actual yield of total naphthoquinones from Xinjiang Lithospermum was 2.0%. The extract had a strong odor and a noticeable off-odor.

[0041] Comparative Example 2: (1) Raw material pretreatment: Take Xinjiang purple gromwell (root) dried at 50℃ and crush it through a 30-mesh sieve.

[0042] (2) First stage of extraction: 1 kg of sieved material was loaded into a supercritical extraction vessel, and 1.5 kg of 95% ethanol was added as an entrainer. Extraction was carried out for 1.5 h at the following conditions: pressure of extraction vessel: 8 MPa, temperature: 50 ℃, CO2 flow rate: 30 L / h, pressure of separation vessel I: 6 MPa, temperature of separation vessel I: 35 ℃, pressure of separation vessel II: 4 MPa, temperature of separation vessel II: 30 ℃. At this time, the material liquid released from separation vessel II was 105.5 g of Xinjiang Lithospermum extract. Second stage of extraction: The pressure of the supercritical extraction vessel was adjusted to 35 MPa, temperature: 50 ℃, CO2 flow rate: 50 L / h, and extraction was carried out for 2 h. At this time, the extraction was fully completed. The entrainer was transferred to separation vessel I. The material liquid in separation vessel I was collected and concentrated to dryness in a rotary evaporator at 50 ℃ to obtain Xinjiang Lithospermum extract.

[0043] Detection: Total naphthoquinones from Xinjiang Lithospermum were detected by high performance liquid chromatography. Eight components, namely shikonin, isovaleroshikonin, acetylshikonin, deoxyshikonin, β-hydroxyisovaleroshikonin, β,β-dimethylacryloylacanine, isobutyryloylshikonin, and β-acetoxyisovaleroylacanine, were quantitatively detected. The actual yield of total naphthoquinones from Xinjiang Lithospermum was 3.5%. The overall odor was strong and had a noticeable foul smell.

[0044] Comparative Example 3: (1) Raw material pretreatment: Take Xinjiang purple gromwell (root) dried at 50℃ and crush it through a 30-mesh sieve.

[0045] (2) Step 1: 1 kg of pretreated material was placed in an extraction tank, and 10 kg of 95% ethanol aqueous solution was added for soaking and extraction for 24 h. After filtration, the residue was soaked and extracted again with 8 kg of 95% ethanol aqueous solution for 24 h. After filtration, the residue was soaked and extracted again with 8 kg of 95% ethanol aqueous solution for 24 h. After filtration, the three filtrates were combined and concentrated to dryness using a rotary evaporator at 50 degrees Celsius to obtain Xinjiang Lithospermum extract. High performance liquid chromatography (HPLC) was used to quantitatively detect eight components: shikonin, isovaleryl shikonin, acetyl shikonin, deoxyshikonin, β-hydroxyisovaleryl shikonin, β,β-dimethylacryloyl argentin, isobutyryl shikonin, and β-acetoxyisovaleryl argentin. The total naphthoquinone yield was calculated to be 2.78%. GC-MS was used to quantitatively detect volatile components. The overall odor was strong and had a noticeable foul smell, indicating a high content of volatile components. According to the appendix... Figure 1 (Example 1) and Appendix Figure 2 (Comparative Example 3) Compared with Comparative Example 3, the peaks with retention times of 7.622, 7.967, 9.859, and 12.686 in Example 1 are presumably isovaleric acid, ethyl octanoate, ethyl decanoate, and ethyl palmitate, respectively, and their peak areas decreased (the peak areas in Example 1 were 479337, 41468, 32694, and 120230, respectively; the peak areas in Comparative Example 3 were 774540, 534900, 377872, and 828875, respectively). According to the peak area ratio of these four absorption peaks, the content of volatile components in Example 1 is 61.9%, 7.8%, 8.7%, and 14.5% of that in Comparative Example 3, respectively, indicating that the content of volatile components in Example 1 is reduced.

[0046] Test Example 1: Evaluation of Anti-aging Effect Human skin fibroblasts in the logarithmic growth phase were harvested, digested, resuspended, and seeded into 6-well cell culture plates, with three replicates per group. The plates were incubated at 37°C in a 5% CO2 environment. When the cells reached approximately 80% confluence, H2O2 was added to treat the cells and induce senescence. Then, samples containing the formulations from each example and comparative example were added, with the naphthoquinone content adjusted to 0.78 μg / mL. Group BC served as the blank control group, and group NC served as the model group. The cells were cultured for another 3 days, after which the supernatant was discarded, and the cells were fixed. After staining with β-galactosidase (β-gal), the cells were observed under a microscope, with at least 100 cells per field of view. The β-gal positivity rate of each group was calculated.

[0047] The formula for calculating the β-gal positivity rate is: β-gal (%) = number of positive cells in the field of view / total number of cells in the field of view × 100%, see Table 1.

[0048] Table 1

[0049] Conclusion: The extracts of Lithospermum erythrorhizon from Xinjiang using different extraction processes in the examples can all significantly reduce H2O2-induced cell senescence, and the effects of the extracts of Lithospermum erythrorhizon in the examples are significantly better than those in the comparative examples.

[0050] Test Example 2: Evaluation of Antioxidant Effect Immortalized human keratinocytes (HaCaT) in the logarithmic growth phase were harvested, digested, resuspended, and seeded into 24-well cell culture plates, with three replicates per group. Cells were incubated overnight at 37°C in a 5% CO2 environment to ensure full cell adhesion (70% confluence). Pretreatment with culture medium containing 200 μg / ml of different samples was then performed, followed by H2O2 treatment to establish an oxidative damage model. After 1 day of further culture, the supernatant was discarded, and the cells were incubated with 20 μM 2',7'-dichlorodihydrofluorescein diacetate (DCFH-DA) staining solution for 20 min. The staining solution was removed, and the cells were washed twice with PBS. Cells were digested, centrifuged, and resuspended in PBS. The relative fluorescence intensity (RFI) of each group was measured using a microplate reader. R (See Table 2).

[0051] Table 2

[0052] Conclusion: The extracts of Lithospermum erythrorhizon from Xinjiang using different extraction processes in the examples can all significantly inhibit the generation of ROS in keratinocytes, indicating that they have good antioxidant effects. Moreover, the inhibitory effect of the extracts of Lithospermum erythrorhizon in the examples is significantly better than that of the comparative examples.

[0053] Test Example 3: Evaluation of Anti-ferromorbidity Effect Human keratinocytes in the logarithmic growth phase were harvested, digested, resuspended, and seeded into 24-well cell culture plates containing spreaders, with three replicates per group. The cells were cultured at 37 °C in a 5% CO2 environment. When the cells reached approximately 50% confluence, they were irradiated with UVB at a single dose of 20 mJ, followed by the addition of culture medium containing 200 μg / ml of different samples. After 3 days of repeated irradiation, the supernatant was discarded, and the cells were fixed. The relative fluorescence intensity of glutathione peroxidase 4 (GPX4) in each group was detected by immunofluorescence antibody incubation and fluorescence microscopy, as shown in Table 3.

[0054] Table 3

[0055] Conclusion: The extracts of Lithospermum erythrorhizon from Xinjiang using different extraction processes in the examples can all protect the expression of GPX4 in skin keratinocytes induced by UVB, indicating that they can protect the skin and reduce the ferroptosis effect caused by photoaging. Moreover, the effects of the extracts of Lithospermum erythrorhizon in the examples are significantly better than those in the comparative examples.

[0056] Test Example 4: Sensory Evaluation Test Sensory evaluation tests were conducted on all samples according to GB / T 14454.2-2008. Seven trained evaluators were assigned to evaluate the aroma of six samples, including three example samples and three comparative samples. Each example sample was paired with one of the three comparative samples to form an evaluation group, for a total of nine groups. Before the evaluation, the moderator prepared four clean, odorless scent identification papers for each group, each labeled with a unique code. Two of the papers were dipped into the comparative sample, and the other two into the example sample, with a dip depth of approximately 1 cm to ensure consistent absorption. The four scent identification papers were then mixed crosswise, and one paper was randomly removed. The remaining three papers were placed on a scent identification paper holder and given to the evaluators for independent smelling. Each evaluator identified the group with the lowest odor from the three scent identification papers. Each group of samples underwent three rounds of evaluation, corresponding to the top note, middle note, and base note, with a 10-minute interval between each round. During the evaluation, the evaluators did not discuss with each other, and the moderator only recorded the code of the selected scent identification paper in each round. Each round of identification of the example group as the low-odor group is counted as one correct answer, and the results are recorded in Table 4. According to the critical value (12 times) for 7 evaluators in GB / T 14454.2-2008, if the number of correct judgments does not exceed 12 times, it is determined that there is no significant difference in aroma between the two groups and it is within the acceptable range. If it reaches or exceeds 13 times, it is determined that there is a significant difference in the odor intensity between the two groups of samples and it exceeds the acceptable range.

[0057] Table 4

[0058] Conclusion: The results of the triangular evaluation method show that, compared with the comparative examples, the number of evaluations that identified the lower odor of the three examples was higher than the evaluation threshold, indicating that the overall odor intensity of the three examples was lower than that of the three comparative examples, showing a significant difference.

[0059] The liquid chromatography results of the proportions of each component in the eight naphthoquinone substances of each embodiment are shown in Table 5. The liquid chromatograms of the naphthoquinone from Xinjiang prepared in Example 1 and Comparative Example 3 are shown in Table 5. Figure 4 and Figure 5 .

[0060] Table 5

[0061] It should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit it. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all such modifications or substitutions should be covered within the scope of the claims of the present invention.

Claims

1. A method for preparing a low-odor Xinjiang Lithospermum extract, characterized in that, Includes the following steps: (1) Raw material pretreatment: The raw material of Xinjiang purple gromwell is dried and crushed to obtain pretreated material; (2) First stage extraction: The pretreated material is loaded into a supercritical extraction device, a composite entrainer is added, extraction is carried out, and the first fraction is collected in the first separator; The composite entrainer comprises a lipid material and an alcohol solvent, wherein the lipid material is selected from at least one of glyceryl monostearate, glyceryl 1,3-distearate, and ethyl oleate; (3) Second stage extraction: After the first stage extraction is completed, the second fraction rich in naphthoquinones is collected in the second separator; (4) Post-processing: The second fraction is concentrated to remove the alcohol solvent, and the low-odor Xinjiang Lithospermum extract is obtained.

2. The preparation method according to claim 1, characterized in that, In step (2), the alcohol solvent is an aqueous ethanol solution with a volume concentration of 95% or anhydrous ethanol; the extraction is carried out at an extraction pressure of 8-15 MPa and an extraction temperature of 40-50℃.

3. The preparation method according to claim 2, characterized in that, In the composite entrainer, the mass ratio of the lipid material to the alcohol solvent is 1:1-4.

4. The preparation method according to claim 1, characterized in that, In step (2), the first stage extraction is carried out for 1-2 hours under the condition of CO2 flow rate of 20-30 L / h.

5. The preparation method according to claim 1 or 4, characterized in that, In step (2), the pressure of the first separator is 4-5 MPa and the temperature is 30-35 ℃.

6. The preparation method according to any one of claims 1-4, characterized in that, In step (3), the second stage of extraction involves adjusting the extraction pressure to 30-40 MPa and extracting for 2-3 hours at an extraction temperature of 40-50 ℃ and a CO2 flow rate of 40-50 L / h.

7. The preparation method according to any one of claims 1-4, characterized in that, In step (4), the concentration is carried out by rotary evaporation at 40-60°C.

8. The preparation method according to any one of claims 1-4, characterized in that, In step (1), the drying temperature is 40-60℃; the pulverization is pulverizing to pass through a 20-40 mesh sieve.

9. The Xinjiang Lithospermum extract prepared by the method for preparing low-odor Xinjiang Lithospermum extract according to claim 1, characterized in that, The active ingredient in the Xinjiang Lithospermum extract includes naphthoquinones, which include shikonin, isovaleroshikonin, acetylshikonin, deoxyshikonin, β-hydroxyisovaleroshikonin, β,β-dimethylacryloylacanine, isobutyryloylshikonin, and β-acetoxyisovaleroylacanine.

10. The use of the Xinjiang Lithospermum extract according to claim 9 in the preparation of cosmetics for anti-skin aging, anti-oxidation and / or anti-skin cell ferroptosis.

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