Cistanche deserticola moisture recovery method based on evaporation, cistanche deserticola rotary evaporation recovery water and application

Abstract

The invention belongs to the technical field of biological medicine, and discloses a method for recycling moisture of cistanche based on evaporation, cistanche rotary evaporation recycled water and application, the method comprises the following steps: selecting, cleaning, wiping and cutting cistanche, drying the cistanche by adopting rotary evaporation drying, and recycling moisture generated in the process to obtain the cistanche rotary evaporation recycled water. According to the method, the comprehensive utilization rate of the cistanche drying process is increased, the application field of food and medicine homologous agricultural product processing by-products is expanded, a new solution is provided for green sustainable development of the food industry, the problems of waste water recycling and reutilization in the food and medicine homologous agricultural product drying process are solved, and the method is suitable for industrial production. And a new technical route is provided for active ingredient recovery and resource cyclic utilization of cistanche deserticola.

Description

Technical Field

[0001] This invention belongs to the field of biomedical technology, and in particular to a method for recovering water from Cistanche deserticola by evaporation, the rotary evaporation of Cistanche deserticola to recover water, and its application. Background Technology

[0002] Cistanche deserticola, also known as Cistanche tubulosa, is a perennial herbaceous medicinal material that parasitizes the roots of desert plants. It is mainly produced in arid regions such as Xinjiang and Inner Mongolia. It is sweet, salty, and warm in nature, and has the effects of tonifying kidney yang, nourishing essence and blood, and moistening the intestines to relieve constipation. Cistanche deserticola is rich in active ingredients such as phenylethyl glycosides, iridoids, and polysaccharides. It is a precious tonic medicinal material listed in the *Pharmacopoeia of the People's Republic of China*, mainly containing phenylethyl glycosides such as acteoside and echinacoside. Acteoside is primarily responsible for clearing oxidative waste from the body, reducing inflammation, and protecting the brain and nerves, making the body less prone to aging, inflammation, or damage. Its effect is more focused on "repairing and maintaining bodily stability." Echinacoside, on the other hand, excels at improving physical strength and endurance, reducing fatigue, and helping kidney function and energy recovery; therefore, it is often considered a key component for tonifying the kidneys and enhancing physical strength. In addition, it also has certain neuroprotective effects.

[0003] The molecular structures of verbascoside (A) and echinacoside (B) are as follows: To enhance efficacy or improve user experience, Cistanche deserticola often requires processing (preparation). Fresh Cistanche deserticola retains the most complete components and has a strong laxative effect, but it is cold and damp in nature and difficult to preserve. Alcoholic products, by enhancing the medicinal properties with alcohol, can significantly strengthen its kidney-tonifying effect, making it suitable for those with yang deficiency, but some components may be reduced. Steamed Cistanche deserticola has a better taste and a more prominent laxative effect, making it suitable for dietary supplementation, but high temperatures can reduce some components. Salted products can guide the medicine to the kidneys and enhance kidney-tonifying power, making them suitable for those with kidney deficiency and lower back and knee weakness, but the increased salt content requires caution. Black steaming (similar to nine steaming and nine sun-drying) makes the medicinal properties more gentle and the tonifying effect more lasting, suitable for tonifying applications, but the process is complex and the price is higher. Fermented Cistanche deserticola is a modern process that can improve absorption and flavor, but the quality varies greatly between different manufacturers and still requires further research. In general, different processing methods result in different emphases of medicinal properties; the appropriate form can be chosen based on kidney tonification, laxative effects, or individual constitution. Existing technical literature largely focuses on the separation and quantification of active ingredients in Cistanche deserticola, its water extracts, or alcohol extracts. However, few studies have addressed the chemical components and recovery potential of the water evaporated during processing. Rotary evaporation, a commonly used mild evaporation method in laboratories, is characterized by low temperature, high efficiency, and strong controllability, making it highly suitable for research on the recovery of heat-sensitive active ingredients. Quantitative analysis of verbascoside and echinacoside in the rotary evaporation water will contribute to the development of a new resource recovery method, providing a basis for the full utilization of the components of traditional Chinese medicine. Therefore, it is necessary to develop a method that can systematically recover moisture from Cistanche deserticola and determine the content of verbascoside and echinacoside in the recovered water to evaluate the utilization value of this resource during processing.

[0004] By comparison, the following patent publications related to this invention patent application were found: Comparison Patent 1: Chinese patent publication CN215403654U (A Pig Farm Wastewater Recycling System Based on Rotary Evaporation and Ammonia Recovery Technology) proposes a system for the energy and resource utilization of pig farm wastewater using a three-stage synergistic treatment technology of biogas engineering, vacuum rotary evaporation, and membrane separation ammonia removal. The system consists of a wastewater collection tank, biogas engineering equipment, vacuum rotary evaporation concentration equipment, membrane separation ammonia removal equipment, concentrated liquid packaging equipment, and an ammonium sulfate collection tank. Its workflow is as follows: First, the collected wastewater is sent to the biogas engineering system for anaerobic fermentation, producing biogas and biogas slurry; then, the biogas slurry enters the vacuum rotary evaporation equipment for concentration, obtaining highly concentrated organic fertilizer and condensate; the condensate then enters the membrane separation ammonia removal equipment to remove ammonia ions, generating an ammonium sulfate solution. Simultaneously, the ammonia removal condensate produced can be reused for pig farm cleaning, achieving water resource recycling. This system not only produces biogas, organic fertilizer, and ammonium sulfate as byproducts but also reduces wastewater discharge, possessing both environmental protection and water-saving value.

[0005] The defects are: (1) The system has a complex structure, a large number of equipment, and high construction costs; (2) Ammonia recovery requires the addition of sulfuric acid, which raises concerns about the cost and safety of chemical reagents; (3) The system has high technical requirements for operators; (4) The product quality of the concentrate and ammonium sulfate depends on the composition of the original wastewater and has poor stability; (5) Membrane separation equipment is easily contaminated, leading to a decrease in efficiency.

[0006] A comparison reveals a fundamental difference between this invention and the aforementioned patent publications. This invention focuses on the biomedical processing of Cistanche deserticola, a food-medicine homologous raw material. It utilizes rotary evaporation technology to recover condensate during the drying process and determines functional active ingredients such as verbascoside and echinacoside, aiming to improve resource utilization in the drying process and realize the high-value and edible application of by-products. The condensate obtained by this invention not only retains the plant's natural aroma and some nutritional activity but can also be used in food or daily chemical product formulations, solving the problems of effective ingredient loss and waste of condensate by-products in traditional drying processes. Neither of the two comparative documents addresses the recovery of plant active ingredients, the acquisition of edible condensate, quantitative analysis of functional components, or the resource utilization of by-products from food-medicine homologous agricultural products, nor does it provide any technical inspiration pointing in this direction. Therefore, this invention differs fundamentally from the comparative documents in terms of technical objectives, process route, and practical applications, and belongs to an independent innovative technology system. Summary of the Invention

[0007] The purpose of this invention is to overcome the shortcomings of the prior art and provide a method for recovering water from Cistanche deserticola by evaporation, the method for recovering water from Cistanche deserticola by rotary evaporation, and its application.

[0008] The technical solution adopted by this invention to solve its technical problem is: A method for recovering moisture from Cistanche deserticola based on evaporation, the method comprising selecting, washing, drying and cutting the Cistanche deserticola, and using rotary evaporation to dry the Cistanche deserticola and recover the moisture generated during the process, to obtain Cistanche deserticola rotary evaporation recovered water.

[0009] Furthermore, the specific steps are as follows: (1) Selecting the fruit: Select fresh, disease-free Cistanche deserticola; (2) Cleaning: Use running water to clean the surface of Cistanche deserticola; (3) Drying: After washing, remove excess moisture from the surface of Cistanche deserticola until it is dry; (4) Cutting: Separate the fresh Cistanche deserticola into upper and lower parts. The upper part is the top of the Cistanche deserticola from the top down to 50% of its total height, and the lower part is the root of the Cistanche deserticola from the root up to 50% of its total height. Then cut into 1 cm pieces. 1 cm 1 cm small pieces; (5) Evaporation: Turn on the refrigeration and water bath heating of the rotary evaporator half an hour in advance to 40 ℃~60 ℃, and ensure that the condensation temperature is maintained at 4±1 ℃; weigh the chopped Cistanche deserticola into the rotary flask (keep the weight consistent for each experiment), then install the rotary evaporation system, maintain the vacuum degree at 10±2 kPa, and the rotary evaporation time is 3 h~12 h to obtain the rotary evaporation water of Cistanche deserticola.

[0010] Furthermore, the Cistanche deserticola mentioned is the desert Cistanche deserticola produced in Turpan, Xinjiang.

[0011] Furthermore, the upper part of the fresh desert Cistanche deserticola contains 11.67 μg / mL of verbascoside and 65.79 μg / mL of echinacoside; the lower part contains 5.35 μg / mL of verbascoside and 51.49 μg / mL of echinacoside.

[0012] Furthermore, in step (3), kitchen paper towels are used to absorb excess moisture from the surface of the Cistanche deserticola. Alternatively, in step (5), the rotary evaporator model is EV400H, with a power of 100 W, a rotation speed of 120 rpm, and a vacuum degree of 10±2 kPa.

[0013] Furthermore, in step (5), the content of verbascoside in the rotary evaporation water of Cistanche deserticola is 6.44-32.49 μg / L, and the content of echinacoside is 3.81-7.13 μg / L.

[0014] Furthermore, in step (5), the refrigeration and water bath heating are turned on to 50 °C, and the rotary evaporation time is 9 h.

[0015] Furthermore, in step (5), the content of verbascoside in the rotary evaporation water of Cistanche deserticola is 32.49 μg / L in the upper part and 11.29 μg / L in the lower part, and the content of echinacoside is 6.96 μg / L in the upper part and 7.13 μg / L in the lower part.

[0016] The water from the Cistanche deserticola prepared by the method described above is recovered by rotary evaporation.

[0017] The above describes the application of Cistanche deserticola rotary evaporation water recovery in the daily chemical industry.

[0018] The advantages and positive effects of this invention are as follows: 1. This invention utilizes evaporation (rotary evaporation) to recover water during the processing of Cistanche deserticola and measures the content of verbascoside and echinacoside in the recovered water. This method can be used for the resource utilization of Cistanche deserticola by-products and the recovery of functional substances. The resulting condensate retains its natural aroma and nutritional activity. This invention not only improves the comprehensive utilization rate of the Cistanche deserticola drying process but also expands the application field of by-products from the processing of food and medicinal homologous agricultural products. It provides a new solution for the green and sustainable development of the food industry, solves the problems of wastewater resource utilization and reuse in the drying process of food and medicinal homologous agricultural products, and provides a new technical route for the recovery and resource recycling of effective components from Cistanche deserticola.

[0019] 2. Significantly improves the comprehensive utilization rate of resources in the drying process of Cistanche deserticola: This invention is the first to systematically determine and verify that a certain amount of verbascoside and echinacoside are still present in the water recovered by rotary evaporation, proving that these phenylethyl glycoside active ingredients can migrate with the aqueous phase and be effectively enriched during the drying process. A reliable quantitative analysis method was established by high performance liquid chromatography, providing a scientific basis for evaluating the loss and transfer of effective components during processing.

[0020] 3. Establishing the dynamic distribution law of rotary evaporation time and active ingredient migration: This invention systematically revealed the dynamic change trend of verbascoside and echinacoside in recycled water using different rotary evaporation times as variables. It was found that both exhibited a "first increase then decrease" pattern, and it was clarified that moderate rotary evaporation time is beneficial for the enrichment of active ingredients. This study provides a quantifiable and predictable theoretical basis for optimizing rotary evaporation drying parameters.

[0021] 4. Achieving quantitative detection and scientific evaluation of active ingredients in recycled water: This invention is the first to systematically determine and verify that rotary evaporation recycled water still contains a certain amount of verbascoside and echinacoside, proving that these phenylethyl glycoside active ingredients can migrate with the aqueous phase and be effectively enriched during the drying process. A reliable quantitative analysis method was established using high-performance liquid chromatography, providing a scientific basis for evaluating the loss and transfer of active ingredients during processing.

[0022] 5. Providing reverse guidance for optimizing the drying process of Cistanche deserticola: This invention innovatively uses "content of active ingredients in the recovered water" as an evaluation index to guide the optimization design of drying process conditions (such as temperature and time). This not only helps to reduce the thermal degradation and loss of effective ingredients, but also maximizes the preservation of the medicinal value of Cistanche deserticola while ensuring the quality of drying, thus achieving a dual improvement in processing quality and functional preservation.

[0023] 6. Expanding the high-value application of Cistanche deserticola by-products: The rotary evaporation recovery water obtained by this invention retains certain natural component characteristics and functional material basis, and can be further used for the development of raw materials for food, beverage or daily chemical products. This changes the traditional approach of treating drying condensate as wastewater treatment and provides a new technical path for the resource utilization and high-value utilization of Cistanche deserticola processing by-products.

[0024] 7. The process is mild and safe, with good prospects for promotion: This invention adopts rotary evaporation, a mature and controllable low-temperature evaporation technology. It does not rely on organic solvents or complex chemical treatments. The process is relatively simple and safe, and it is easy to implement in the laboratory and pilot-scale conditions. It also has the potential to be promoted and applied to other food and medicine homologous Chinese medicinal materials or fruit and vegetable raw materials.

[0025] 8. Meets the industrial needs of green processing and sustainable development: By reducing wastewater discharge, improving the utilization rate of by-products and reducing the environmental burden, this invention aligns with the current development direction of green manufacturing and recycling in the food and traditional Chinese medicine processing fields. It has positive significance in terms of both ecological and social benefits and provides a new technological demonstration for the sustainable development of the industry. Attached Figure Description

[0026] Figure 1 This is a schematic diagram of the structural connection of a rotary evaporator in the prior art; wherein, the reference numerals are: 1, condenser tube; 2, feed valve; 3, vacuum gauge; 4, controller; 5, evaporator head; 6, rotating flask; 7, collection flask; 8, discharge valve; 9, water bath; 10, low temperature cooling circulation pump; 11, circulating water vacuum pump; Figure 2 This is the standard curve of verbascoside in this invention; Figure 3 This is the standard curve of echinacoside in this invention; Figure 4 This is a graph showing the verbascoside content in the water recovered from the upper part of Cistanche deserticola at 50 ℃ in this invention. The uppercase letters indicate significant differences in the verbascoside content in the water recovered from the upper part of Cistanche deserticola at different times at 50 ℃. P <0.05); Figure 5 This is a graph showing the verbascoside content in the water recovered from the lower part of Cistanche deserticola at 50 ℃ in this invention. The uppercase letters indicate significant differences in the verbascoside content in the water recovered from the lower part of Cistanche deserticola at different times at 50 ℃. P <0.05); Figure 6 This is a graph showing the echinacoside content in the water recovered from the upper part of Cistanche deserticola at 50 ℃ in this invention. The uppercase letters indicate significant differences in the echinacoside content in the water recovered from the upper part of Cistanche deserticola at different times at 50 ℃. P<0.05); Figure 7 This is a graph showing the echinacoside content in the water recovered from the lower part of Cistanche deserticola at 50 ℃ in this invention. The uppercase letters indicate significant differences in the echinacoside content in the water recovered from the lower part of Cistanche deserticola at different times at 50 ℃. P <0.05); Figure 8 This is a graph showing the verbascoside content in the water recovered from the upper part of Cistanche deserticola at 40 ℃ in this invention. The uppercase letters represent significant differences in the verbascoside content in the water recovered from the upper part of Cistanche deserticola at different times at 40 ℃. P <0.05); Figure 9 This is a graph showing the verbascoside content in the water recovered from the lower part of Cistanche deserticola at 40 ℃ in this invention. The uppercase letters indicate significant differences in the verbascoside content in the water recovered from the lower part of Cistanche deserticola at different times at 40 ℃. P <0.05); Figure 10 This is a graph showing the echinacoside content in the water recovered from the upper part of Cistanche deserticola at 40 ℃ in this invention. The uppercase letters indicate significant differences in the echinacoside content in the water recovered from the upper part of Cistanche deserticola at different times at 40 ℃. P <0.05); Figure 11 This is a graph showing the echinacoside content in the water recovered from the lower part of Cistanche deserticola at 40 ℃ in this invention. The uppercase letters indicate significant differences in the echinacoside content in the water recovered from the lower part of Cistanche deserticola at different times at 40 ℃. P <0.05); Figure 12 This is a graph showing the verbascoside content in the water recovered from the upper part of Cistanche deserticola at 60 ℃ in this invention. The uppercase letters indicate significant differences in the verbascoside content in the water recovered from the upper part of Cistanche deserticola at different times at 60 ℃. P < 0.05); Figure 13 This is a graph showing the verbascoside content in the water recovered from the lower part of Cistanche deserticola at 60 ℃ in this invention. The uppercase letters indicate significant differences in the verbascoside content in the water recovered from the lower part of Cistanche deserticola at different times at 60 ℃. P < 0.05); Figure 14 The graph shows the echinacoside content in the water recovered from the upper part of Cistanche deserticola at 60℃ in this invention. The uppercase letters indicate significant differences in the echinacoside content in the water recovered from the upper part of Cistanche deserticola at different times at 60℃. P <0.05); Figure 15This is a graph showing the echinacoside content in the water recovered from the lower part of Cistanche deserticola at 60 ℃ in this invention. The uppercase letters indicate significant differences in the echinacoside content in the water recovered from the lower part of Cistanche deserticola at different times at 60 ℃. P <0.05); Figure 16 This is a graph showing the verbascoside content in the water recovered from the upper part of Cistanche deserticola at different temperatures after 9 hours, where uppercase letters indicate significant differences in the verbascoside content in the water recovered from the upper part of Cistanche deserticola at different temperatures after 9 hours. P < 0.05); Figure 17 This is a graph showing the verbascoside content in the water recovered from the lower part of Cistanche deserticola at different temperatures after 9 hours, where uppercase letters represent significant differences in the verbascoside content in the water recovered from the lower part of Cistanche deserticola at different temperatures after 9 hours. P < 0.05); Figure 18 This is a graph showing the echinacoside content in the rotary evaporation water from the upper part of Cistanche deserticola at different temperatures after 9 hours, where uppercase letters represent significant differences in echinacoside content in the rotary evaporation water from the upper part of Cistanche deserticola at different temperatures after 9 hours. P < 0.05); Figure 19 This is a graph showing the echinacoside content in the rotary evaporation water from the lower part of Cistanche deserticola at different temperatures after 9 hours, where uppercase letters represent significant differences in the echinacoside content in the rotary evaporation water from the lower part of Cistanche deserticola at different temperatures after 9 hours. P < 0.05). Detailed Implementation

[0027] The present invention will be further described below with reference to the embodiments. The following embodiments are descriptive and not limiting, and should not be used to limit the scope of protection of the present invention.

[0028] The various experimental operations involved in the specific embodiments are all conventional techniques in the field. For parts not specifically annotated in this document, those skilled in the art can refer to various commonly used reference books, scientific and technological documents or related instructions and manuals prior to the filing date of this invention to carry out the operations.

[0029] A method for recovering moisture from Cistanche deserticola based on evaporation, the method comprising selecting, washing, drying and cutting the Cistanche deserticola, and using rotary evaporation to dry the Cistanche deserticola and recover the moisture generated during the process, to obtain Cistanche deserticola rotary evaporation recovered water.

[0030] Furthermore, the specific steps are as follows: (1) Selecting the fruit: Select fresh, disease-free Cistanche deserticola; (2) Cleaning: Use running water to clean the surface of Cistanche deserticola; (3) Drying: After washing, remove excess moisture from the surface of Cistanche deserticola until it is dry; (4) Cutting: Separate the fresh Cistanche deserticola into upper and lower parts. The upper part is the top of the Cistanche deserticola from the top down to 50% of its total height, and the lower part is the root of the Cistanche deserticola from the root up to 50% of its total height. Then cut into 1 cm pieces. 1 cm 1 cm small pieces; (5) Evaporation: Turn on the refrigeration and water bath heating of the rotary evaporator half an hour in advance to 40 ℃~60 ℃, and ensure that the condensation temperature is maintained at 4±1 ℃; weigh the chopped Cistanche deserticola into the rotary flask (keep the weight consistent for each experiment), then install the rotary evaporation system, maintain the vacuum degree at 10±2 kPa, and the rotary evaporation time is 3 h~12 h to obtain the rotary evaporation water of Cistanche deserticola.

[0031] Furthermore, the Cistanche deserticola mentioned is the desert Cistanche deserticola produced in Turpan, Xinjiang.

[0032] Furthermore, the upper part of the fresh desert Cistanche deserticola contains 11.67 μg / mL of verbascoside and 65.79 μg / mL of echinacoside; the lower part contains 5.35 μg / mL of verbascoside and 51.49 μg / mL of echinacoside.

[0033] Furthermore, in step (3), kitchen paper towels are used to absorb excess moisture from the surface of the Cistanche deserticola. Alternatively, in step (5), the rotary evaporator model is EV400H, with a power of 100 W, a rotation speed of 120 rpm, and a vacuum degree of 10±2 kPa.

[0034] Furthermore, in step (5), the content of verbascoside in the rotary evaporation water of Cistanche deserticola is 6.44-32.49 μg / L, and the content of echinacoside is 3.81-7.13 μg / L.

[0035] Furthermore, in step (5), the refrigeration and water bath heating are turned on to 50 °C, and the rotary evaporation time is 9 h.

[0036] Furthermore, in step (5), the content of verbascoside in the rotary evaporation water of Cistanche deserticola is 32.49 μg / L in the upper part and 11.29 μg / L in the lower part, and the content of echinacoside is 6.96 μg / L in the upper part and 7.13 μg / L in the lower part.

[0037] The water from the Cistanche deserticola prepared by the method described above is recovered by rotary evaporation.

[0038] The above-mentioned applications of Cistanche deserticola rotary evaporation water recovery in the food and / or daily chemical industries.

[0039] The present invention adopts the following technical solution: A rotary steaming processing method for desert Cistanche deserticola involves selecting, washing, drying, and cutting the Cistanche deserticola, and then using rotary steaming to dry the Cistanche deserticola and recover the water generated during the process. The recovered water is obtained by rotary steaming of Cistanche deserticola. The contents of verbascoside and echinacoside in the recovered water are determined by high performance liquid chromatography and compared with the contents of substances obtained by rotary steaming Cistanche deserticola at different temperatures.

[0040] The relevant rotary evaporation in this invention can be used as follows: Figure 1 The rotary evaporator shown is used for this process.

[0041] Specifically, the relevant preparation and testing methods are as follows: Example 1 Fresh, disease-free Cistanche deserticola from the Xinjiang desert was selected (the upper part of fresh desert Cistanche deserticola contained 11.67 μg / g of verbascoside and 65.79 μg / g of echinacoside; the lower part contained 5.35 μg / g of verbascoside and 51.49 μg / g of echinacoside. All other examples were the same). The surface of the Cistanche deserticola was thoroughly cleaned with running water. After cleaning, excess moisture was absorbed using kitchen paper towels until dry. The Cistanche deserticola was then separated into upper and lower parts. The upper part consisted of the top of the Cistanche deserticola extending downwards to 50% of its total height, and the lower part consisted of the root extending upwards to 50% of its total height. The pieces were then cut into 1 cm pieces. 1cm For 1 cm pieces, perform the following treatment: Rotary evaporation for 3 h, 6 h, 9 h, and 12 h: The rotary evaporator (model: EV400H, power: 100 W, speed: 120 rpm) was preheated by turning on the cooling and water bath heating to 50 °C half an hour in advance, ensuring the condensation temperature remained at 4 ± 1 °C. 150 g of the chopped Cistanche deserticola was weighed and placed in a rotary flask, and then the rotary evaporation system was installed (any system known in the art can be used, such as...). Figure 1 The equipment shown is identical in all other embodiments. The vacuum degree is maintained at 10±2 kPa, and the rotary evaporation time is 3 h, 6 h, 9 h, and 12 h to obtain the rotary evaporation water from Cistanche deserticola.

[0042] The contents of echinacoside and verbascoside were determined by high performance liquid chromatography (General Chapter 0512, Chinese Pharmacopoeia 2025). Chromatographic grade verbascoside and echinacoside were prepared into standard solutions with a concentration of 10 mg / mL. The standards were serially diluted with 50% methanol (v / v, volume percentage) to 4.8828 μg / L and 2.4414 μg / L, respectively, and the peak areas were measured. A standard curve was plotted with the standard concentration (μg / mL) on the x-axis and the peak area on the y-axis, and linear regression was performed: Verascoside standard curve: y = 72350x + 15390, R0 2 =0.9998 ( Figure 2 Echinacoside standard curve: y = 36505x + 92800, R 2 =0.9995 ( Figure 3 ).

[0043] The rotary evaporated water was filtered through a 0.22 μm organic filter membrane, and the contents of verbascoside and echinacoside were determined by high performance liquid chromatography (HPLC). Chromatographic column: Kromasil C18 (250 mm × 4.6 mm, 5 μm); column temperature: 30 ℃; injection volume: 20 μL; phase A: aqueous solution containing 0.1% acetic acid, phase B: acetonitrile containing 0.1% acetic acid; flow rate: 1 mL / min. The solvent elution gradient for phase B was: 0 min–2 min: 5%, 2 min–4 min: 5%–15%, 4 min–12 min: 15%–25%, 12 min–18 min: 25%–35%, 18 min–20 min: 35%–100%, 20 min–23 min: 100%, 23 min–23.5 min: 100%–5%, 23.5 min–26 min: 5%. The detection wavelength was 330 nm and the injection volume was 20 μL.

[0044] like Figure 4 As shown in the figure, under rotary evaporation conditions at 50 ℃, the content of verbascoside in the upper part of the Cistanche deserticola recovery water showed a trend of first increasing and then decreasing with the extension of rotary evaporation time. The figure shows that the verbascoside content was 26.82 μg / L after 3 h of rotary evaporation. With the extension of rotary evaporation time to 6 h and 9 h, the content increased significantly, reaching a maximum of 32.49 μg / L at 9 h, which was significantly higher than other time points. P<0.05). When the rotary evaporation time was further extended to 12 h, its content decreased significantly. This phenomenon indicates that in the early to middle stages of rotary evaporation, as water continues to evaporate and the system volume decreases, verbascoside, as a hydrophilic phenylethanol glycoside, is easily migrated with the aqueous phase and enriched, thus exhibiting a concentration effect; while prolonged heating may cause some verbascoside to undergo thermal degradation or structural instability, thereby causing its content to decrease.

[0045] like Figure 5 As shown, the content of verbascoside in the water recovered from the lower part of Cistanche deserticola also showed a pattern of first increasing and then decreasing with the rotary evaporation time. At 3 h of rotary evaporation, the content was 8.37 μg / L. With the extension of rotary evaporation time to 6 h and 9 h, the content of verbascoside gradually increased, reaching its highest value (11.29 μg / L) at 9 h, significantly higher than other treatment times. P <0.05). When the rotary evaporation time was extended to 12 h, its content decreased significantly. Overall, the content of verbascoside in the lower part of the recovered water was significantly lower than that in the upper part, but the trend was consistent. This may be related to the denser tissue structure and higher degree of lignification in the lower part of Cistanche deserticola, which makes the migration efficiency of verbascoside to the aqueous phase during rotary evaporation lower, thus resulting in a lower overall content in the recovered water.

[0046] like Figure 6 As shown, under rotary evaporation at 50 ℃, the echinacoside content in the upper part of Cistanche deserticola recovered water also showed a trend of first increasing and then decreasing with the evaporation time. The echinacoside content was 5.35 μg / L after 3 h of rotary evaporation. As the evaporation time was extended to 6 h and 9 h, the content gradually increased, reaching a maximum value (6.96 μg / L) at 9 h, significantly higher than other time points. P <0.05). When the rotary evaporation time was extended to 12 h, its content decreased. Compared with verbascoside, the content of echinacoside in the recycled water was generally lower, and the response range to rotary evaporation time was smaller. This may be related to its lower initial content and relatively poor thermal stability, making it more prone to degradation or transformation under long-term heating conditions.

[0047] like Figure 7As shown, the echinacoside content in the water recovered from the lower part of Cistanche deserticola showed a similar trend to that in the upper part with rotary evaporation time, but the overall content level and variation range were smaller. The echinacoside content was 5.73 μg / L after 3 h of rotary evaporation. After extending the evaporation time to 6 h and 9 h, the content gradually increased, reaching a maximum of 7.13 μg / L at 9 h. When the rotary evaporation time was further extended to 12 h, the content decreased to 6.17 μg / L. These results indicate that the migration and accumulation of echinacoside in the lower tissue during rotary evaporation are also significantly affected by the evaporation time. However, due to the limitations of the tissue structure, its release efficiency is lower than that in the upper tissue, and it is more susceptible to thermal effects under longer heating times.

[0048] Example 2 Fresh, pest-free Cistanche deserticola from the Xinjiang desert was selected. The surface of the Cistanche deserticola was thoroughly washed with running water. After washing, excess moisture was absorbed using kitchen paper towels until dry. The Cistanche deserticola was then divided into upper and lower parts. The upper part consisted of the top of the Cistanche deserticola extending downwards to 50% of its total height, while the lower part consisted of the root extending upwards to 50% of its total height. The pieces were then cut into 1 cm pieces. 1 cm For 1 cm pieces, perform the following treatment: Rotary evaporation for 3 h, 6 h, 9 h, and 12 h: The rotary evaporator (model: EV400H, power: 100 W, speed: 120 rpm) was preheated with cooling and water bath heating at 40 ℃ for half an hour to ensure the condensation temperature remained at 4±1 ℃. 150 g of the chopped Cistanche deserticola was weighed and placed in a rotary flask. The rotary evaporation system was then installed, maintaining a vacuum of 10±2 kPa. The evaporation times were 3 h, 6 h, 9 h, and 12 h, yielding the Cistanche deserticola rotary evaporation recovery water.

[0049] The methods for determining the content of verbascoside and echinacoside are the same as in Example 1.

[0050] like Figure 8 As shown, under rotary evaporation conditions at 40 ℃, the content of verbascoside in the upper part of the Cistanche deserticola recovery water showed a trend of first increasing and then decreasing with the extension of rotary evaporation time. At 3 h of rotary evaporation, the content was 24.47 μg / mL, significantly lower than other treatment times. With the extension of rotary evaporation time to 6 h and 9 h, the verbascoside content significantly increased, reaching relatively high and similar levels at 6 h and 9 h (26.5 μg / L and 26.55 μg / L, respectively), with no significant difference between the two, but significantly higher than at 3 h and 12 h. P<0.05). When the rotary evaporation time was extended to 12 h, its content decreased to 25.16 μg / L. This result indicates that under relatively mild conditions of 40℃, the middle stage of rotary evaporation (6 h and 9 h) is conducive to the enrichment of verbascoside in the recovered water, while excessively long rotary evaporation may lead to a decrease in content due to a reduced concentration rate or loss of some components.

[0051] like Figure 9 As shown, the content of verbascoside in the water recovered from the lower part of Cistanche deserticola also showed a trend of first increasing and then decreasing with rotary evaporation time, but the overall content was significantly lower than that in the upper part. At 3 h of rotary evaporation, the content was 7.81 μg / mL, significantly lower than at other time points. With the extension of rotary evaporation time to 6 h, the content increased to 9.07 μg / L, and further increased significantly at 9 h, reaching a maximum (10.41 μg / L). When the rotary evaporation time was extended to 12 h, the content decreased to 8.72 μg / L. This phenomenon may be related to the denser structure of the lower part and the slower release rate of the active ingredients. Extending the rotary evaporation time helps verbascoside gradually migrate to the aqueous phase, but excessively long rotary evaporation is not conducive to its further enrichment.

[0052] like Figure 10 As shown, under rotary evaporation at 40 ℃, the echinacoside content in the upper part of Cistanche deserticola recovered water exhibited significant stage-wise changes with increasing evaporation time. At 3 h of evaporation, the content was 4.69 μg / L, significantly lower than at other time points. With evaporation time extended to 6 h, the content increased to 5.06 μg / L, and further increased significantly at 9 h, reaching a maximum of 5.67 μg / L. When the evaporation time was extended to 12 h, the content decreased to approximately 5.14 μg / L. These results indicate that under 40 ℃ conditions, echinacoside can gradually accumulate with the aqueous phase during rotary evaporation, but its accumulation efficiency decreases with longer evaporation times, possibly related to its relatively low thermal stability.

[0053] like Figure 11 As shown, the trend of echinacoside content in the recovered water from the lower part of Cistanche deserticola was basically the same as that from the upper part, but the overall content and the magnitude of change were slightly lower. The content was 5.08 μg / L after 3 h of rotary evaporation, significantly lower than that after 6 h, 9 h, and 12 h. With the extension of rotary evaporation time to 6 h, the content increased to 5.34 μg / L, reaching a maximum of 6.15 μg / L at 9 h. When the rotary evaporation time was extended to 12 h, the content decreased to 5.33 μg / L. These results indicate that rotary evaporation time is an important factor affecting the recovery of echinacoside from the lower part, but due to the tissue structure and initial content limitations, its enrichment degree in the recovered water is still lower than that of the upper tissue.

[0054] Example 3 Fresh, pest-free Cistanche deserticola from the Xinjiang desert was selected. The surface of the Cistanche deserticola was thoroughly washed with running water. After washing, excess moisture was absorbed using kitchen paper towels until dry. The Cistanche deserticola was then divided into upper and lower parts. The upper part consisted of the top of the Cistanche deserticola extending downwards to 50% of its total height, while the lower part consisted of the root extending upwards to 50% of its total height. The pieces were then cut into 1 cm pieces. 1 cm For 1 cm pieces, perform the following treatment: Rotary evaporation for 3 h, 6 h, 9 h, and 12 h: The rotary evaporator (model: EV400H, power: 100 W, speed: 120 rpm) was preheated with cooling and water bath heating at 60 ℃ for half an hour to ensure the condensation temperature remained at 4±1 ℃. 150 g of the chopped Cistanche deserticola was weighed and placed in a rotary flask. The rotary evaporation system was then installed, maintaining a vacuum of 10±2 kPa. The evaporation times were 3 h, 6 h, 9 h, and 12 h, yielding the Cistanche deserticola rotary evaporation recovery water.

[0055] The methods for determining the content of verbascoside and echinacoside are the same as in Example 1.

[0056] like Figure 12 As shown, under rotary evaporation conditions at 60 ℃, the content of verbascoside in the upper part of the Cistanche deserticola recovery water showed a trend of first increasing and then decreasing with the extension of rotary evaporation time. After 3 h of rotary evaporation, its content was 20.15 μg / L, significantly lower than that of other treatment times (…). P <0.05). When the rotary evaporation time was extended to 6 h and 9 h, the content of verbascoside increased significantly, reaching high levels at 6 h and 9 h (21.82 μg / L and 21.87 μg / L, respectively), with no significant difference between the two, but significantly higher than at 3 h and 12 h. With further extension of the rotary evaporation time to 12 h, its content decreased to 20.72 μg / L. This result indicates that at a higher temperature of 60 ℃, the middle stage of rotary evaporation is conducive to the enrichment of verbascoside in the recovered water, while excessively long rotary evaporation may cause thermal degradation or structural damage of some verbascoside due to high temperature, thus leading to a decrease in its content.

[0057] like Figure 13 As shown, the content of verbascoside in the water recovered from the lower part of Cistanche deserticola also showed a trend of first increasing and then decreasing with rotary evaporation time, but the overall content was significantly lower than that in the upper part. After 3 hours of rotary evaporation, its content was 6.44 μg / L, significantly lower than that at other treatment times (…). P<0.05). With increasing rotary evaporation time to 6 h, its content increased to 7.47 μg / L, and further increased significantly at 9 h, reaching a maximum of 8.57 μg / L. When the rotary evaporation time was extended to 12 h, its content decreased to 7.18 μg / L. These results indicate that verbascoside in the lower tissue can also gradually migrate and accumulate with the aqueous phase during rotary evaporation. However, due to the dense tissue structure and limited release of active ingredients, its content in the recovered water is consistently lower than that in the upper tissue, and it is more susceptible to thermal effects under high-temperature, long-term rotary evaporation conditions.

[0058] like Figure 14 As shown, under rotary evaporation at 60 ℃, the echinacoside content in the upper part of Cistanche deserticola recovered water exhibited significant stage-wise changes with increasing rotary evaporation time. After 3 h of rotary evaporation, the content was 3.81 μg / L, significantly lower than that at other treatment times (…). P <0.05). With increasing rotary evaporation time to 6 h, the content increased to 4.11 μg / L, and further increased significantly at 9 h, reaching a maximum of 4.61 μg / L. When the rotary evaporation time was extended to 12 h, the content decreased to 4.18 μg / L. This trend indicates that in the initial and middle stages of rotary evaporation, water evaporation leads to the continuous enrichment of echinacoside in the recovered water. However, under higher temperatures and longer rotary evaporation times, echinacoside may undergo some degradation due to its relatively poor thermal stability, resulting in a decrease in content.

[0059] like Figure 15 As shown, the trend of echinacoside content in the water recovered from the lower part of Cistanche deserticola with rotary evaporation time was basically the same as that in the upper part, but the overall content and the range of change were relatively small. At 3 h of rotary evaporation, the content was 4.12 μg / L, significantly lower than that at 6 h, 9 h, and 12 h. P <0.05). With increasing rotary evaporation time to 6 h, the content increased to 4.34 μg / L, reaching a maximum of 5.00 μg / L at 9 h. When the rotary evaporation time was extended to 12 h, the content decreased to 4.33 μg / L. These results indicate that rotary evaporation time significantly affects the recovery of echinacoside from the lower part of the tissue. However, due to the denser structure and lower release efficiency of the active ingredient in the lower tissue, its enrichment in the recovered water is significantly weaker than that of the upper tissue, and its content is more likely to decline under high-temperature, long-term rotary evaporation conditions.

[0060] Under 9-hour rotary evaporation conditions, different temperatures significantly affected the verbascoside content in the water recovered from both the upper and lower parts of Cistanche deserticola. Overall, the verbascoside content showed a pattern of first increasing and then decreasing with increasing rotary evaporation temperature. Figure 16As shown, for the upper part of the Cistanche deserticola sample, the verbascoside content in the rotary evaporation recovery water was 26.55 μg / L at 40 ℃. When the temperature was increased to 50 ℃, the content increased significantly and reached a maximum of 32.49 μg / L, which was 5.94 μg / L higher than that at 40 ℃. However, when the temperature was further increased to 60 ℃, the verbascoside content decreased significantly to only 21.87 μg / L, which was 10.62 μg / L lower than that at 50 ℃, indicating that excessively high temperatures are not conducive to the retention of this component in the recovery water.

[0061] like Figure 17 As shown, the variation trend of the lower part of Cistanche deserticola samples is consistent with that of the upper part, but the overall content level is significantly lower. At 40 ℃, the verbascoside content was 10.41 μg / L; it increased to 11.29 μg / L at 50 ℃, reaching its highest value; when the temperature increased to 60 ℃, it decreased to 8.57 μg / L, a reduction of 2.72 μg / L compared to 50 ℃, indicating that high temperature also leads to the loss of verbascoside in the lower part of the sample. Comparing different parts, at the same rotary evaporation temperature, the verbascoside content in the water recovered from the rotary evaporation of the upper part of Cistanche deserticola was consistently significantly higher than that of the lower part. For example, at 50 ℃, the content in the upper part was 32.49 μg / L, while that in the lower part was only 11.29 μg / L, approximately 2.8 times higher in the upper part. This is closely related to the higher accumulation of active ingredients in the lower part of the tissue.

[0062] Under 9-hour rotary evaporation conditions, the changes in echinacoside content in the water recovered from the upper and lower parts of Cistanche deserticola were consistent with the trends of verbascoside, both showing a "first increase, then decrease" trend with increasing temperature, with a peak at 50 ℃. Figure 18 As shown, for the upper part of Cistanche deserticola, the echinacoside content in the recovered water was 5.67 μg / L at 40 ℃. The content reached its highest level of 6.96 μg / L at 50 ℃, an increase of 1.29 μg / L compared to 40 ℃. Further heating to 60 ℃ resulted in a significant decrease in the content to 4.61 μg / L, a reduction of 2.35 μg / L compared to 50 ℃. This indicates that moderate heating is beneficial for echinacoside to enter the recovered water in the upper part of the sample, but excessively high temperatures will lead to a reduction in its recovery.

[0063] like Figure 19 As shown, for the lower part of Cistanche deserticola, the echinacoside content was 6.15 μg / L at 40 ℃, reaching a maximum of 7.13 μg / L at 50 ℃ (an increase of 0.98 μg / L compared to 40 ℃). When the temperature rose to 60 ℃, it decreased to about 5.00 μg / L (a decrease of 2.13 μg / L compared to 50 ℃). This also exhibited a pattern of first increasing and then decreasing, and 50 ℃ was most favorable for the accumulation of echinacoside in the recycled water.

[0064] From the perspective of part-specific differences, at the same temperature, the echinacoside content in the lower part of the recycled water is generally higher than that in the upper part: for example, at 40 ℃, the lower part is 6.15 μg / L and the upper part is 5.67 μg / L; at 50 ℃, the lower part is 7.13 μg / L and the upper part is 6.96 μg / L; and at 60 ℃, the lower part is 5.00 μg / L and the upper part is 4.61 μg / L. This difference is usually related to the tissue structure and component distribution of different parts of Cistanche deserticola. The lower part often accumulates more active ingredients, and therefore a higher amount enters the recycled water during rotary evaporation. The main reason for this trend is the "dual effect" of temperature. In the 40-50 ℃ range, increased temperature promotes the dissolution and mass transfer of echinacoside in cell tissues, making it easier for it to enter the recycled water with water vapor condensation, thus increasing its content. However, when the temperature rises to 60 ℃, echinacoside may undergo a certain degree of thermal degradation / structural instability. At the same time, high temperature may also lead to adsorption and loss in the rotary evaporation system, ultimately resulting in a decrease in its content in the recycled water.

[0065] Meanwhile, by comparing Examples 1 to 3, it can be seen that the rotary evaporation conditions of 9 h and the rotary evaporation temperature of 50°C in the method of the present invention have a synergistic effect, which can synergistically increase the content of verbascoside and echinacoside in the recovered water of the prepared Cistanche deserticola. In particular, it can synergistically increase the content of verbascoside and echinacoside in the upper part recovered water of the prepared Cistanche deserticola, and the content of verbascoside and echinacoside in the lower part recovered water of the prepared Cistanche deserticola.

[0066] In existing technologies, methods such as freeze drying, vacuum drying, reduced-pressure cold air drying, microwave vacuum drying, and infrared vacuum drying focus on "moisture removal," which are usually accompanied by the destruction of material structure and composition due to heat or prolonged exposure. In contrast, rotary evaporation drying technology directly evaporates moisture by reducing pressure at a lower temperature. This not only preserves the original form, active ingredients, and flavor of the material to the greatest extent possible, but also efficiently condenses and recovers the moisture that has escaped from the material, achieving a dual leap in drying quality and resource recovery.

[0067] Furthermore, in existing technologies, rotary evaporation is mainly used for the concentration and solvent recovery of active ingredients in extracts of medicinal and edible herbs or natural products. Its core technical objective is to reduce solvent usage, increase the concentration of target components, or achieve solvent recycling. In such technical solutions, the liquid condensed during rotary evaporation is usually considered "recovered solvent" or "waste liquid requiring further treatment." Evaluation indicators mainly focus on solvent recovery rate, extraction efficiency, target product purity, or concentration factor, without considering the composition and functional value of the recovered water itself. In the field of medicinal herb processing, especially in the processing and drying of medicinal and edible herbs, rotary evaporation is almost never used to systematically recover the water evaporated from the raw materials themselves, let alone to quantitatively analyze and evaluate the active ingredients in this water.

[0068] Although embodiments of the invention have been disclosed for illustrative purposes, those skilled in the art will understand that various substitutions, variations, and modifications are possible without departing from the spirit and scope of the invention and the appended claims. Therefore, the scope of the invention is not limited to the contents disclosed in the embodiments.

Claims

1. A method for recovering moisture from Cistanche deserticola based on evaporation, characterized in that: The method includes selecting, washing, drying, and cutting Cistanche deserticola, and using rotary evaporation to dry Cistanche deserticola and recover the water generated during the process to obtain Cistanche deserticola rotary evaporation water. The specific steps are as follows: (1) Selecting the fruit: Select fresh, disease-free Cistanche deserticola; (2) Cleaning: Use running water to clean the surface of Cistanche deserticola; (3) Drying: After washing, remove excess moisture from the surface of Cistanche deserticola until it is dry; (4) Cutting: Separate the fresh Cistanche deserticola into upper and lower parts. The upper part is the top of the Cistanche deserticola from the top down to 50% of its total height, and the lower part is the root of the Cistanche deserticola from the root up to 50% of its total height. Then cut into 1 cm pieces. 1 cm 1 cm small pieces; (5) Evaporation: Turn on the refrigeration and water bath heating of the rotary evaporator half an hour in advance to 40 ℃~60 ℃, and ensure that the condensation temperature is maintained at 4±1 ℃; weigh the chopped Cistanche deserticola into the rotary flask, keep the weight consistent for each experiment, then install the rotary evaporation system, maintain the vacuum degree at 10±2 kPa, and the rotary evaporation time is 3 h~12 h to obtain the rotary evaporation water of Cistanche deserticola.

2. The method according to claim 1, characterized in that: The Cistanche deserticola mentioned is Cistanche aridans.

3. The method according to claim 2, characterized in that: The upper part of the desert Cistanche deserticola contained 11.67 μg / mL of verbascoside and 65.79 μg / mL of echinacoside; the lower part contained 5.35 μg / mL of verbascoside and 51.49 μg / mL of echinacoside.

4. The method according to claim 1, characterized in that: In step (3), kitchen paper towels are used to absorb excess moisture from the surface of the Cistanche deserticola. Alternatively, in step (5), the rotary evaporator has a power of 100 W, a rotation speed of 120 rpm, and a vacuum degree of 10±2 kPa.

5. The method according to any one of claims 1 to 4, characterized in that: In step (5), the content of verbascoside in the rotary evaporation water of Cistanche deserticola is 6.44-32.49 μg / L and the content of echinacoside is 3.81-7.13 μg / L.

6. The method according to claim 1, characterized in that: In step (5), turn on the refrigeration and water bath heating to 50 °C, and the rotary evaporation time is 9 h.

7. The method according to claim 6, characterized in that: In step (5), the content of verbascoside in the rotary evaporation water of Cistanche deserticola was 32.49 μg / L in the upper part and 11.29 μg / L in the lower part, and the content of echinacoside was 6.96 μg / L in the upper part and 7.13 μg / L in the lower part.

8. The water recovered by rotary evaporation of Cistanche deserticola prepared by the method according to any one of claims 1 to 7.

9. The application of the Cistanche deserticola rotary evaporation water recovery method as described in claim 8 in the daily chemical industry.

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