Thermosensitive traditional Chinese medicine powder sterilization process

Abstract

The invention relates to the technical field of traditional Chinese medicine powder sterilization, and provides a thermosensitive traditional Chinese medicine powder sterilization process which comprises the following steps: S100, preparing a sterilization medium which is prepared from the following components in percentage by weight: 10-12% of EO and the balance of CO2; s200, a sterilization medium is introduced into a modulation container with the design pressure being 0.3 MPa, and the gas pressure value in the modulation container reaches 0.2 MPa; s300, the sterilization medium in the preparation container is introduced into a sterilization container containing the traditional Chinese medicine powder to be treated, the concentration of EO in the sterilization container is controlled to be 200 mg / L-400 mg / L, aiming at thermosensitive traditional Chinese medicine powder, the residual amount of EO in the sterilized traditional Chinese medicine powder is reduced, and the use safety of traditional Chinese medicine is improved; 90% of CO can reduce the explosion risk of EO and improve the safety of the sterilization process; the whole sterilization process can be completed within 8-12 hours, so that the sterilization efficiency is improved; on the premise that the requirement for killing microorganisms is met, the original form and color of the medicine powder can be kept unchanged, the change amplitude of the water content of the medicine powder is small, and the retention rate of core effective components is high.

Description

TECHNICAL FIELD

[0001] Embodiments of the present application relate to the technical field of traditional Chinese medicine powder sterilization, in particular, to a heat-sensitive traditional Chinese medicine powder sterilization process. BACKGROUND

[0002] Heat-sensitive traditional Chinese medicine contains effective components (such as volatile oil, glycosides) that are easily volatile, oxidized or decomposed by heat. Its sterilization process needs to ensure microbial killing effect while avoiding damage to the medicinal ingredients. At present, according to the Chinese Pharmacopoeia and industry practice, the sterilization methods of different forms of heat-sensitive traditional Chinese medicine are different. For heat-sensitive traditional Chinese medicine powder, cobalt 60 irradiation sterilization method is often selected. However, the existing mainstream sterilization methods still have the following significant defects: 1. Although cobalt 60 has strong penetration, it takes a long time to sterilize, which cannot meet the rapid processing needs of large quantities of products; 2. The half-life of cobalt 60 isotope is 5.27 years, and the radiation capacity decays over time, so the radioactive source needs to be replaced regularly, and the management cost is high; 3. The radioactive source needs to be strictly supervised. The operator needs to wear a dosimeter and receive regular radiation safety training to ensure personal dose compliance. The protection facilities meet the radiation protection standards, and the safety management is complex; 4. Moreover, the replacement and maintenance of the radioactive source require the intervention of professional institutions, further increasing the operating cost; 5. This method requires different sterilization doses for different items and is difficult to accurately control, which can easily cause chemical changes in traditional Chinese medicine, resulting in changes in the content of effective substances. The content of effective substances is not the total amount of traditional Chinese medicine powder, but the amount of specific active chemical components in traditional Chinese medicine powder that are directly related to therapeutic efficacy and have been confirmed by modern pharmacological research. These components are the core material basis for traditional Chinese medicine powder to exert efficacy, and their content directly determines the strength of the efficacy. The gamma rays of cobalt 60 can destroy the chemical structure of these components, resulting in a decrease in their total amount or loss of activity, ultimately leading to changes in the content of effective substances.

[0003] For example, the effective substance of safflower seed powder is safflower volatile oil (containing alpha-thujone, eucalyptol, etc.), which has the functions of opening the orifice, regulating qi, and anti-inflammatory, and is a key ingredient for treating cough and asthma. The high-energy rays of cobalt 60 irradiation can destroy the carbon-carbon double bond and ether bond of volatile oil, causing volatile oil to decompose into inactive small molecule compounds, ultimately reducing the content of safflower volatile oil.

[0004] The effective substance of Sanqi powder is notoginseng saponin (such as R1, Rg1, Rb1), which has the functions of promoting blood circulation to remove blood stasis, anti-platelet aggregation, and improving microcirculation. Cobalt 60 irradiation can break the glycoside bond of notoginseng saponin, separate the aglycone from the sugar, and generate inactive aglycone fragments, resulting in a significant decrease in the total content of notoginseng saponin, especially the active monomers Rg1 and Rb1.

[0005] The effective substances of amber powder are amber glycosides and resin glycosides, which have the effects of calming the nerves, promoting blood circulation and removing blood stasis. Irradiation can destroy the cyclic structure of glycosides, resulting in a decrease in the content of amber glycosides and a decrease in the drug efficacy.

[0006] In addition, in the sterilization of traditional Chinese medicines, there is also a method of using ethylene oxide for sterilization, for example, a new type of traditional Chinese medicine residue treatment process disclosed in Chinese patent application No. CN107319996A mentioned that after the metered medicinal materials are crushed to 10-20 mesh, they are placed in a sealed container and sterilized with ethylene oxide or ozone for 30 minutes. This scheme is mainly for the raw medicinal materials of cold decoction preparations. However, for heat-sensitive traditional Chinese medicine powders, such as amber powder, safflower fruit and sanchi powder, which contain volatile oil and glycosides, if pure ethylene oxide is used for sterilization, it will result in a high residual amount of EO in the traditional Chinese medicine powder, and EO is easy to react with phenolic and glycoside components in heat-sensitive traditional Chinese medicine powder, resulting in darkening and yellowing of the powder. For example, the color of safflower fruit powder changes from light green to yellowish brown, and the uniformity of the color of the traditional Chinese medicine powder is easily destroyed. Local color spots may appear due to the difference in the residual concentration of EO. In addition, the scheme mentioned that medicinal ethanol with an ethanol content of 5-95% or water is used as a solvent for soaking until it is transparent, and then it is stored for 24-48 hours. Amber powder, sanchi powder and other traditional Chinese medicines contain natural pigments (such as flavonoid pigments in sanchi powder and resin pigments in amber powder). The specific surface area of the powder is large, and the contact with water and ethanol is more sufficient. A large amount of pigments will dissolve into the soaking liquid, resulting in a significant change in the color of the traditional Chinese medicine powder itself (for example, the color of sanchi powder changes from yellowish white to grayish white, and the color of amber powder changes from brownish yellow to light brown). In addition, the moisture content of heat-sensitive traditional Chinese medicine powder needs to be controlled. If soaking treatment is used, the powder will be in a high moisture state for a long time, which may also induce the degradation of heat-sensitive components, such as the hydrolysis of glycosides.

[0007] For example, Chinese patent application No. CN104127768A mentioned a traditional Chinese medicine composition for treating high viscosity blood syndrome, which mentioned that the various raw materials treated in steps a-g were dried at a temperature of 50-60℃ for 4-6 hours, and then were crushed and sieved through an 80-mesh sieve. The crushed raw materials were weighed according to the ratio of the traditional Chinese medicine composition of claim 1, mixed uniformly, sterilized with ethylene oxide, and finally encapsulated with a No. 1 capsule plate to obtain a capsule dosage form for treating high viscosity blood syndrome. The method implemented in this scheme includes a combination of various traditional Chinese medicine components, and the overall stability is higher than that of pure heat-sensitive powder such as amber powder and sanchi powder. If pure ethylene oxide is used for sterilization of heat-sensitive traditional Chinese medicines such as amber powder, sanchi powder and safflower fruit according to the content disclosed in this document, it may also result in a large amount of toxic gas remaining in the sterilized traditional Chinese medicine product, and pure ethylene oxide is easy to react with the components of heat-sensitive traditional Chinese medicine powder, resulting in changes in the content of the substances. In addition, the humidity required by pure ethylene oxide as a sterilization medium is easy to cause the caking of heat-sensitive traditional Chinese medicine powder and changes in the color of the sterilized product.

[0008] For example, the Chinese invention patent CN1620868A, concerning ethylene oxide sterilizing gas, mentions ethylene oxide as the main disinfection and sterilization component. This component has strong penetrating power in gas mixtures, effectively killing various bacterial vegetative cells, spores, viruses, and fungal spores. It can undergo non-specific alkylation reactions with the proteins, DNA, and RNA of microorganisms, rendering them inactive and achieving a sterilization effect. However, it also explicitly states that it is suitable for disinfection and sterilization of various fields and various items (excluding food). This is because dichlorodifluoromethane and methyl bromide are toxic to humans, and the core purpose of this solution is to stabilize the EO concentration and prevent combustion and explosion, guiding technical personnel to explore the sterilization stability of the sterilizing gas on items rather than its potential sterilization of edible pharmaceuticals. Summary of the Invention

[0009] To overcome the above-mentioned defects, the present invention provides a sterilization process for heat-sensitive traditional Chinese medicine powder, which solves the technical problem of a sterilization process for heat-sensitive traditional Chinese medicine powder in related technologies / existing technologies.

[0010] According to one aspect, at least one embodiment of the present invention provides a sterilization process for heat-sensitive traditional Chinese medicine powder, comprising the following steps: S100: Configure sterilization media, wherein the sterilization media consists of the following components by weight percentage: EO: 10%, with the balance being CO2; S200: The sterilization medium is introduced into a conditioning container with a design pressure of 0.3 MPa, and the gas pressure inside the conditioning container reaches 0.2 MPa; S300: Pass the sterilization medium in the preparation container into the sterilization container containing the Chinese medicine powder to be processed, and control the concentration of EO in the sterilization container at 200mg / L~400mg / L.

[0011] For example, in a heat-sensitive traditional Chinese medicine powder sterilization process provided in at least one embodiment of the present invention, the sterilization medium is composed of the following components by weight percentage: EO: 10%, with the balance being CO2.

[0012] For example, in a heat-sensitive traditional Chinese medicine powder sterilization process provided in at least one embodiment of the present invention, in step S300, the humidity value of the sterilization container is set to 20%~60%RH (±5%), and the temperature of the sterilization container is set to 30℃~60℃.

[0013] The beneficial effects of the embodiments of the present invention are as follows: In this invention, for heat-sensitive Chinese herbal medicine powders, a mixed gas of 10% EO (ethylene oxide) and 90% CO2 (carbon dioxide) by weight is used as the sterilization medium. This reduces the residual EO in the sterilized powder and improves the safety of using the medicine. At the same time, 90% CO2 can reduce the risk of EO combustion and explosion, improving the safety of the sterilization process. The entire sterilization process can be completed within 8 to 12 hours, significantly shortening the sterilization time and improving sterilization efficiency. While ensuring that the requirements for microbial killing are met, the original shape and color of the powder remain unchanged, and the change in the moisture content of the powder is small, resulting in a high retention rate of core effective components. Attached Figure Description

[0014] To more clearly illustrate the technical solutions in the embodiments of the present invention, the accompanying drawings used in the description of the embodiments of the present invention will be briefly introduced below. Obviously, the drawings described below are merely some exemplary embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on the content of the exemplary embodiments of the present invention and these drawings without any creative effort.

[0015] Figure 1 This is a schematic diagram of a heat-sensitive traditional Chinese medicine powder sterilization process in one embodiment of the present invention. Detailed Implementation

[0016] The present invention will now be described in further detail with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and not intended to limit it.

[0017] To keep the drawings concise, each drawing only schematically shows the parts relevant to the invention; these do not represent the actual structure of the product. Furthermore, for ease of understanding, in some drawings, only one of components with the same structure or function is schematically shown, or only one is labeled. In this document, "one" not only means "only one," but can also mean "more than one," and "several" includes "two" and "more than two."

[0018] In this document, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to fixed connections, detachable connections, or integral connections; they can refer to mechanical connections or electrical connections; they can refer to direct connections or indirect connections through an intermediate medium; and they can refer to the internal communication between two components. Those skilled in the art can understand the specific meaning of the above terms in this invention based on the specific circumstances.

[0019] In this invention, unless otherwise explicitly specified and limited, "above" or "below" the second feature can include direct contact between the first and second features, or contact between the first and second features through another feature between them. Furthermore, "above," "over," and "on top" of the second feature includes the first feature directly above or diagonally above the second feature, or simply indicates that the first feature is at a higher horizontal level than the second feature. "Below," "below," and "under" the second feature includes the first feature directly below or diagonally below the second feature, or simply indicates that the first feature is at a lower horizontal level than the second feature.

[0020] In the description of this embodiment, terms such as "upper," "lower," "left," and "right" are based on the orientation or positional relationship shown in the accompanying drawings. They are used only for the convenience of description and simplification of operation, and are not intended to indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on the present invention.

[0021] Furthermore, in the description of this application, the terms "first," "second," etc., are used only to distinguish descriptions and should not be construed as indicating or implying relative importance.

[0022] like Figure 1 As shown in the embodiments provided by the present invention, the sterilization of heat-sensitive traditional Chinese medicine powder adopts the following steps: S100: Configure sterilization media, wherein the sterilization media consists of the following components by weight percentage: EO: 10%~12%, with the balance being CO2; S200: The sterilization medium is introduced into a conditioning container with a design pressure of 0.3 MPa, and the gas pressure inside the conditioning container reaches 0.2 MPa.

[0023] S300: Pass the sterilization medium in the preparation container into the sterilization container containing the Chinese medicine powder to be processed, control the concentration of EO in the sterilization container at 200mg / L~400mg / L, set the humidity of the sterilization container at 20%~60%RH (±5%), and set the temperature of the sterilization container at 30℃~60℃.

[0024] The table below shows the sterilization effect of heat-sensitive Chinese herbal medicine powders under specific temperature, humidity, and EO concentration conditions in a sterilization medium of 10% EO and 90% CO2, using amber powder, Panax notoginseng powder, and Artemisia argyi as examples:

[0025] Based on the above data, the aerobic bacteria count of all three powders after sterilization was ≤10 cfu / g, and the mold and yeast counts of amber powder, Panax notoginseng powder, and Artemisia argyi were all ≤103 cfu / g, which is lower than the standard of "mold ≤10³ cfu / g". Escherichia coli and Salmonella were not detected in any of the three powders, indicating that the mixed medium can specifically kill intestinal pathogens and meet the requirements for sterility and safety in pharmaceuticals.

[0026] The table below compares the residual EO content, powder morphology and color, powder moisture content changes, and active ingredient content of heat-sensitive Chinese medicine powder after sterilization for 4 hours with sterilization media of EO: 10% and CO2: 90% under specific temperature, humidity, and EO concentration conditions with sterilization data of pure ethylene oxide for 1 to 7 days.

[0027]

[0028] Based on the above data, the use of pure ethylene oxide for sterilizing heat-sensitive traditional Chinese medicine powders is explained as follows: Amber powder sterilization results: The amber powder contained high levels of EO residue, resulting in noticeable caking, darkening of color, and the appearance of discoloration. The content of resin glycosides decreased by 20%–40% compared to before sterilization, and this decrease was positively correlated with the EO residue level (280 ppm). Areas with higher EO residue exhibited more severe resin glycoside degradation. In addition to the overall decrease in content, various inactive degradation products were generated, such as alkylated resin derivatives, resin quinones, and free sugars, which may increase the risk of gastrointestinal irritation during oral administration.

[0029] Explanation of Panax notoginseng powder sterilization process: An increase in moisture content of 0.06g~0.09g causes a water film to form on the surface of the Panax notoginseng powder particles, resulting in the particles sticking together under tension. Simultaneously, the 100% EO sterilization process lasts 1~7 days, and the prolonged high-humidity environment further densifies the sticky particles, forming agglomerates with a diameter of 2mm~5mm. After sterilization, the Panax notoginseng powder is no longer a uniform, loose, light yellow fine powder, but rather a mixture of large agglomerates and a small amount of loose powder. The agglomerates are relatively hard and require grinding to disperse, but the original fineness cannot be restored, severely affecting the uniformity of subsequent preparations.

[0030] Explanation of sterilization of Artemisia annua: High EO residues will react with the carbon-carbon double bonds and phenolic hydroxyl groups of volatile oils (such as α-thujone) in Artemisia annua, destroying the conjugated structure of the volatile oils and generating dark alkylated products. For example, the color of thujone changes from light yellow to dark brown after being replaced by EO. A water content of 0.10g~0.15g provides a medium for the oxidation reaction. After the volatile oils come into contact with oxygen, brown aldehydes / ketones are generated. The strong adsorption of Artemisia annua causes EO to form a high concentration area on the surface and inside of the powder particles. The local reaction is more intense, and eventually dark brown irregular spots appear.

[0031] 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 sterilization process for heat-sensitive traditional Chinese medicine powder, characterized in that, Includes the following steps: S100: Configure sterilization media, wherein the sterilization media consists of the following components by weight percentage: EO: 10%~12%, with the balance being CO2; S200: The sterilization medium is introduced into a modulation container with a design pressure of 0.3 MPa, and the gas pressure inside the modulation container reaches 0.2 MPa; S300: The sterilization medium in the preparation container is introduced into a sterilization container containing the Chinese medicine powder to be processed, and the concentration of EO in the sterilization container is controlled at 200mg / L~400mg / L.

2. The sterilization process for heat-sensitive traditional Chinese medicine powder according to claim 1, characterized in that, The sterilization medium consists of the following components by weight percentage: EO: 10%, with the balance being CO2.

3. The sterilization process for heat-sensitive traditional Chinese medicine powder according to claim 2, characterized in that, In step S300, the humidity of the sterilization container is set to 20%~60%RH (±5%), and the temperature of the sterilization container is set to 30℃~60℃.

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