Processing method of traditional Chinese medicine pinellia ternate

Abstract

This invention discloses a method for processing the traditional Chinese medicine Pinellia ternata. The method involves processing the raw Pinellia ternata in a phosphate solution under sealed conditions, followed by slicing into thick pieces and drying to obtain the processed product. The medicinal material is Pinellia ternata or Arisaema heterophyllum. The method of this invention uses phosphate solution to soak Pinellia ternata, which significantly reduces its irritant properties. Toxicological experiments have shown that the processed Pinellia ternata is non-irritating and does not cause a numbing sensation on the tongue. This invention does not use alum, thus avoiding the use of residual Al from alum as a processing excipient in pharmacopoeia methods. 3+ The toxicity to the human nervous system is minimal, ensuring safe and effective clinical use. Compared with traditional processing methods, phosphate-processed Pinellia ternata has the advantages of quantifiable process indicators, simple operation, and no introduction of hazards. It provides a reference for the processing technology of phosphate-processed Pinellia ternata, lays the foundation for the quality stability of phosphate-processed Pinellia ternata, and ensures the safety and efficacy of traditional Chinese medicine.

Description

Technical Field

[0001] This invention belongs to the field of traditional Chinese medicine technology, specifically relating to a method for processing the traditional Chinese medicine Pinellia ternata. Background Technology

[0002] Pinellia ternata (Thunb.) Breit., a plant in the Araceae family, is a dried tuber. It is pungent, warm in nature, and toxic, and enters the spleen, stomach, and lung meridians. It has the effects of drying dampness and resolving phlegm, relieving nausea and vomiting, and dissipating lumps and nodules. It is used for damp phlegm, cold phlegm, cough with excessive phlegm, phlegm-induced dizziness and palpitations, wind-phlegm dizziness, phlegm-induced headache, vomiting and nausea, chest and epigastric fullness, and globus hystericus; externally, it is used to treat carbuncles and phlegm nodules. However, Pinellia ternata is "toxic and irritates the throat." Accidental ingestion of fresh or raw Pinellia ternata can cause numbness and swelling of the mouth and tongue, loss of voice, and difficulty breathing, exhibiting strong irritant toxicity.

[0003] The earliest historical record of the toxicity of Pinellia ternata is found in the "Shennong's Classic of Materia Medica" from the Han Dynasty, which states that "it is highly toxic and should not be taken for a long time." Modern research has found that clinical accidental ingestion can cause swelling and pain of the lips, loss of voice, salivation, spasms, difficulty breathing, and even suffocation and death. Skin contact can cause itching and eczema, and in severe cases, contact dermatitis. It has been reported that Pinellia ternata toxic needle crystal suspension increases the permeability of peritoneal capillaries in mice and the content of inflammatory mediators prostaglandin E2 (PGE2), nitric oxide (NO), and malondialdehyde (MDA) in peritoneal exudate. It also causes paw edema in rats and significantly increases the amount of inflammatory mediators PGE2 and cyclooxygenase-2 (COX-2) in the inflamed paws (Zhu Fagen, Shi Runjun, Yu Hongli, et al. Study on the inflammatory effect of Pinellia ternata toxic needle crystal [J]. Chinese Traditional and Herbal Drugs, 2012, 43(04):739-742). Other studies have shown that Pinellia ternata lectin protein can stimulate macrophages, leading to the release of inflammatory factors such as TNF-α and IL-1β, excessive production of reactive oxygen species (ROS), increased expression of cell receptor interaction protein RIP3, and macrophage necrosis (Yu Hongli, Mao Shanhu, Zhao Tengfei, et al. Gingerol antagonizes the increase in inflammatory factor TNF-α release, excessive ROS production and increased RIP3 expression caused by Pinellia ternata lectin protein stimulation of macrophages [J]. Chinese Journal of Traditional Chinese Medicine, 2015, 40(18):3630-3635; Jin Yangping, Wu Hao, Yu Hongli, et al. Study on the mechanism of gingerol antagonizing the irritant toxicity of Pinellia ternata 'Palm Leaf' needle crystal [J]. Chinese Journal of Traditional Chinese Medicine, 2016, 41(06):1087-1092). Pinellia ternata powder suspension caused severe conjunctival irritation (Cheng Yanqiu, Yu Hongli, Wu Hao, et al. Study on the changes in irritant toxicity of different processed Pinellia ternata products and detection of lectin protein [J]. Chinese Journal of Traditional Chinese Medicine, 2022, 47(17): 4627-4633). In Lei Gong Pao Zhi Lun, it is said that "Pinellia ternata has saliva on it, which causes qi to flow backward and liver qi to be full of anger"; and in Ben Cao Xin Bian, it is said that "Pinellia ternata is dry and scorches yin, and dryness leads to heat, which adds to the heat. Pinellia ternata is a dry medicine, which further consumes the qi in the kidney. Once the qi is consumed, fire will move and water will dry up, and instead of producing essence, phlegm will be produced." Modern research shows that after a single oral administration of a high dose of Pinellia ternata aqueous extract to mice, hepatocytes can exhibit varying degrees of edema, fatty degeneration, and partial punctate necrosis. Simultaneously, serum alanine aminotransferase (ALT) and aspartate aminotransferase (AST) levels show a significant dose-dependent increase, with a prolonged duration of toxicity (Zhang Limei, Bao Zhiye, Huang Youyi, et al. Study on the dose-time-toxicity relationship of Pinellia ternata aqueous extract on mouse hepatotoxicity [J]. Chinese Drug Surveillance, 2011, 8(01): 11-15). Oral administration of high doses of raw Pinellia ternata decoction for 10 days can lead to hepatocyte edema and fatty degeneration in mice; it also causes scattered focal lymphocyte infiltration in the renal parenchyma and cast formation in the renal tubules (Yan Xiaoying, Chen Jupeng, Dong Ju, et al. Toxicity study of raw Pinellia ternata decoction [J]. Information on Traditional Chinese Medicine, 2012, 29(01): 102-105). Therefore, processed Pinellia ternata is often used orally in clinical practice.

[0004] Traditional Chinese medicine (TCM) processing is a pharmaceutical technique based on TCM theory, considering the needs of diagnosis and treatment, the properties of the herbs themselves, and the different requirements of preparation. The processing of Pinellia ternata has a long history, first appearing in the *Huangdi Neijing* (Yellow Emperor's Inner Classic) from the Spring and Autumn and Warring States periods, where it is mentioned as "treating Pinellia ternata." From the Han to the Tang dynasties, the main processing methods included washing with hot water, processing with ginger, boiling, roasting, and baking. For example, the *Jinkui Yuhan Jing* (Golden Chamber Jade Box Classic) from the Han dynasty states: "For Pinellia ternata, do not chew it. Wash it several times with hot water until the water is clear and smooth. If it is not washed thoroughly, it will be poisonous." The *Liu Juanzi Guiyi Fang* (Liu Juanzi's Ghostly Prescriptions) from the Southern Qi dynasty states: "Wash it seven times with hot water, soak it in ginger overnight, and then boil it." The *Bencao Jing Jizhu* (Collected Annotations on the Materia Medica) from the Liang dynasty states: "Boil Pinellia ternata until boiling, change the water three times in this way, then wash it thoroughly. After that, break it into small pieces according to its size and add it to the hot water." Sun Simiao's *Beiji Qianjin Yaofang* (Essential Prescriptions Worth a Thousand Gold Pieces) from the Tang dynasty states: "Roast it over a low flame, grind it into powder, mix it with wine, and take it in doses the size of millet grains." During the Song Dynasty, there were many methods for processing Pinellia ternata, including stir-frying with wheat bran, processing with alum, making koji, processing with ginger and alum, processing with ginger and radish, processing with ginger and licorice, processing with ash, processing with vinegar, and processing with rice. For example, in *Taiping Huimin Heji Jufang*, "processed with alum" is described as "boiled in water for thirty boils, thinly sliced, dried, and stir-fried with ginger juice"; in *Taiping Shenghui Fang*, "washed seven times to remove the slipperiness, stir-fried with wheat bran until slightly yellow"; in *Chuanxin Shiyong Fang*, "washed seven times with water and pounded with ginger to make cakes. Cut into quarters, first wash seven times with water, then mix with large slices of radish, boil over low heat until the taste is no longer offensive, then dry and discard the radish"; in *Leibian Zhu Shi Jiyan Yifang*, "washed ten times with water, stir-fried with sand until hot, sliced, soaked in half a cup of ginger juice, soaked with three qian of licorice root for two or three nights, then dried, soaked and dried again"; in *Nüke Baiwen*, "processed Pinellia ternata" is described as "washed seven times with water, ground into powder, mixed with ginger juice, dried, ground into powder again, mixed with ginger juice again, for a total of seven or eight times. Take and eat until it is not spicy." During the Ming Dynasty, processing methods were added, including processing with Evodia rutaecarpa, processing with soapberry, alum, and ginger, and processing Pinellia ternata according to traditional methods. The Compendium of Materia Medica describes the processing of Pinellia ternata as follows: "Use large Pinellia ternata, wash it seven times with hot water, dry it, wash it again, repeat this process seven times, soak it in thick rice water for one day and one night, add one and a half ounces of alum per ounce, dissolve in warm water and soak for five days, dry it, add one mace of lead oxide, dissolve in warm water and soak for another seven days, boil it in rice water over a low flame, dry it and store it." During the Qing Dynasty, other processing methods emerged, including those using soapberry and alum, ginger, mulberry leaves and salt, croton seeds, and ginger and salt. Through long-term experience and selection, some processing methods for Pinellia ternata are still used today, mainly including alum processing (clear Pinellia ternata), licorice and lime processing (processed Pinellia ternata), ginger and alum processing (ginger Pinellia ternata), and fermentation processing (Pinellia ternata starter). The 2020 edition of the Chinese Pharmacopoeia includes processed Pinellia ternata of clear type, ginger, and processed Pinellia ternata, all of which are processed using the same methods. The processing method for Qingbanxia is as follows: Take clean Pinellia ternata, separate them by size, soak them in an 8% alum solution or boil them until there is no dry core inside and a slightly numbing sensation is felt on the tongue. Remove them, wash them, cut them into thick slices, and dry them. For every 100kg of clean Pinellia ternata, use 12.5kg of alum for the boiling method and 20kg of alum for the soaking method. The processing method for Jiangbanxia is as follows: Take clean Pinellia ternata, separate them by size, soak them in water until there is no dry core inside, remove them; separately, take sliced ​​fresh ginger, decoct it in water, add alum and boil it together with the Pinellia ternata until thoroughly cooked, remove them, and air dry them, or air dry them until semi-dry and then dry them; or cut them into thin slices and dry them. For every 100kg of clean Pinellia ternata, use 25kg of fresh ginger and 12.5kg of alum.The processing method for Pinellia ternata is as follows: Take Pinellia ternata, separate them by size, soak them in water until there is no dry core inside, and remove them. Separately, take an appropriate amount of licorice root, decoct it twice with water, combine the decoctions, pour them into a lime solution made with an appropriate amount of water, stir well, add the soaked Pinellia ternata, and soak it. Stir 1-2 times a day, and keep the pH of the soaking solution above 12, until the cross-section is uniformly yellow and there is a slight numbing sensation on the tongue when tasted. Remove it, wash it, and air-dry or bake it. For every 100 kg of clean Pinellia ternata, use 15 kg of licorice root and 10 kg of quicklime.

[0005] The residue of alum, an auxiliary material used in the processing of Pinellia ternata and Pinellia ternata, can cause Al2O3. 3+ The toxicity to the human nervous system is slow, long-term, and difficult to detect. It forms deposits in the brain, causing neurological lesions, interfering with thinking, consciousness, and memory functions, leading to brain damage, memory decline, and potentially symptoms of Alzheimer's disease. Excessive consumption can cause dermatitis, bronchial asthma, and even affect the metabolism of human cells, causing a series of biochemical reactions to be hindered. To address the above deficiencies, this invention provides a method for processing Pinellia ternata using the food additive phosphate. As a food additive, phosphate is healthier and harmless than alum, as it can dissolve calcium oxalate needle crystals and denature proteins. Summary of the Invention

[0006] The purpose of this invention is to provide a method for processing the traditional Chinese medicine Pinellia ternata. This method is simple, effectively reduces toxicity, and avoids the introduction of new toxic substances.

[0007] The objective of this invention can be achieved through the following technical solutions:

[0008] A method for processing traditional Chinese medicine includes the following steps: processing raw traditional Chinese medicine in a phosphate solution under sealed conditions, then cutting it into thick slices and drying it to obtain processed traditional Chinese medicine; wherein the traditional Chinese medicine is Pinellia ternata or Arisaema heterophyllum.

[0009] As a preferred technical solution, the processing method is as follows (1) or (2) or (3):

[0010] (1) The raw Chinese medicinal materials are soaked in a phosphate solution for 0.5 to 7 days at a temperature of 10 to 100°C; preferably, the raw Chinese medicinal materials are soaked in a phosphate solution for 2 to 6 days at a temperature of 20 to 60°C.

[0011] (2) Soak the raw Chinese medicinal materials in a phosphate solution until there is no white core inside, and then boil for 0.5 to 12 hours; preferably, soak the raw Chinese medicinal materials in a phosphate solution until there is no white core inside, and then boil for 1 to 12 hours.

[0012] (3) Soak the raw Chinese medicine under the conditions described in (1) and then take it out; then boil the ginger slices, phosphate solution and raw Chinese medicine together until thoroughly cooked.

[0013] More preferably, the phosphate is any one or a combination of at least two of sodium hexametaphosphate, sodium pyrophosphate, and sodium tripolyphosphate; the phosphate is used alone or in combination with other excipients.

[0014] More preferably, when the phosphate is a combination of any two of sodium hexametaphosphate, sodium pyrophosphate, and sodium tripolyphosphate, the molar ratio is: sodium hexametaphosphate:sodium tripolyphosphate = 1:100-100:1; sodium hexametaphosphate:sodium pyrophosphate = 1:100-100:1; sodium tripolyphosphate:sodium pyrophosphate = 1:100-100:1; when the phosphate is a combination of sodium hexametaphosphate, sodium pyrophosphate, and sodium tripolyphosphate, the molar ratio is: sodium hexametaphosphate, sodium pyrophosphate, and sodium tripolyphosphate = 2-110:1-100:1-10. More preferably, when the phosphate is a combination of any two of sodium hexametaphosphate, sodium pyrophosphate, and sodium tripolyphosphate, the molar ratio is: sodium hexametaphosphate:sodium tripolyphosphate = 1:10 to 10:1; sodium hexametaphosphate:sodium pyrophosphate = 1:10 to 10:1; sodium tripolyphosphate:sodium pyrophosphate = 1:10 to 10:1; when the phosphate is a combination of sodium hexametaphosphate, sodium pyrophosphate, and sodium tripolyphosphate, the molar ratio is: sodium hexametaphosphate, sodium pyrophosphate, and sodium tripolyphosphate = 30 to 110:5 to 10:1.

[0015] More preferably, the concentration of the phosphate solution is 0.01–1.5 mol / L. Even more preferably, the concentration of the phosphate solution is 0.01–0.7 mol / L.

[0016] More preferably, the ratio of the raw Chinese medicinal product to the phosphate solution (g / ml) is 1:1 to 35.

[0017] The detailed technical solutions of this invention are as follows: Method 1: Place the cleaned raw Pinellia ternata or Arisaema heterophyllum in a sealed container, add phosphate solution at a material-to-liquid ratio (g / mL) of 1:1-35, soak at 10-100℃ for 0.5-7 days, then cut into thick slices and dry to obtain processed Pinellia ternata or Arisaema heterophyllum. Method 2: Place the raw Pinellia ternata or Arisaema heterophyllum in a sealed container, add phosphate solution at a material-to-liquid ratio (g / mL) of 1:1-35, soak until there is no white core inside, then boil for 0.5-12 hours, then cut into thick slices and dry to obtain processed Pinellia ternata or Arisaema heterophyllum. Method 3: After soaking the raw Chinese medicine under the conditions described in Method 1, remove it; then boil ginger slices, phosphate solution, and raw Chinese medicine together thoroughly. The concentration of the phosphate solution is 0.01-1.5 mol / L. In a further embodiment of this invention, the phosphate is any one of sodium hexametaphosphate, sodium pyrophosphate, and sodium tripolyphosphate, or any combination of two or three.

[0018] The evaluation index method for the products of the phosphate-processed Pinellia ternata or Arisaema heterophyllum of the present invention includes determining the content of calcium oxalate needle crystals and determining the similarity of fingerprint spectra.

[0019] (a) The method for determining the content of calcium oxalate needle crystals includes the following steps:

[0020] 1) Chromatographic conditions

[0021] The chromatographic column was SinoPak SP AQ-C18 (250 mm × 4.6 mm, 5 μm), the mobile phase was 0.5% (v / v) phosphoric acid-water, the injection volume was 10 μL, the column temperature was 28℃, the flow rate was 1.0 ml / min, and the detection wavelength was 220 nm.

[0022] 2) Preparation of reference solution

[0023] Accurately weigh 21.18 mg of oxalic acid reference standard, place it in a 10 mL volumetric flask, and dilute to the mark with water to prepare a 1 mL stock solution containing 2.118 mg of oxalic acid reference standard.

[0024] 3) Preparation of the test solution

[0025] Accurately weigh approximately 0.2 g of Pinellia ternata sample powder (passed through a 60-mesh sieve), place it in a centrifuge tube, add 3 mL of ultrapure water and mix well. Heat in a 60°C water bath for 20 min, centrifuge and discard the supernatant. Repeat the above operation once. Add 0.4 mL of concentrated hydrochloric acid solution (volume ratio 1:1) and 3.0 mL of ultrapure water to the residue, mix well, heat in a 60°C water bath for 30 min, centrifuge and collect the supernatant. Place it in a 5 mL volumetric flask and dilute to the mark to obtain the test solution. Filter through a 0.22 μm microporous membrane for later use.

[0026] 4) Plotting the standard curve

[0027] Accurately pipette an appropriate amount of the oxalic acid reference standard stock solution prepared in step 2), and dilute it with water to prepare a series of solutions with concentrations of 10.59 μg / mL, 52.95 μg / mL, 105.90 μg / mL, 158.85 μg / mL, 211.80 μg / mL, and 264.75 μg / mL, respectively. Inject these solutions according to the HPLC chromatographic conditions described in step 1). Plot a standard curve with concentration (μg / mL) on the x-axis (X) and peak area (mAU*min) on the y-axis (Y). (The oxalic acid standard curve is shown in Figure 1). Figure 1 (As shown).

[0028] (II) The method for determining fingerprint similarity includes the following steps:

[0029] 1) Chromatographic conditions

[0030] The chromatographic column was SinoPak SP AQ-C18 (250 mm × 4.6 mm, 5 μm), the mobile phase was acetonitrile (A) - 0.1% (v / v) formic acid - water (B), the injection volume was 10 μL, the column temperature was 30 °C, the flow rate was 1.0 ml / min, the detection wavelength was 260 nm, and the gradient elution program was as shown in Table 1 of Example 7.

[0031] 2) Preparation of the test solution

[0032] Accurately weigh 1.0g of Pinellia ternata powder (passed through a 60-mesh sieve), place it in an Erlenmeyer flask, add 20ml of 50% (v / v) methanol, seal tightly, soak for 30min, sonicate for 1h, filter, take 15ml of the filtrate, evaporate to dryness, add water to make up to 2ml in a volumetric flask, shake well, and filter through a 0.22μm microporous membrane to obtain the final product.

[0033] The beneficial effects of this invention are:

[0034] The method of this invention uses phosphate solution to soak Pinellia ternata, which can significantly reduce its irritant properties. Toxicological experiments have shown that the processed Pinellia ternata is non-irritating and does not cause a numbing sensation on the tongue. This invention does not use alum, thus avoiding the use of residual Al from alum as a processing excipient in pharmacopoeia methods. 3+ The toxicity to the human nervous system is minimal, ensuring safe and effective clinical use. Compared with traditional processing methods, phosphate-processed Pinellia ternata has the advantages of quantifiable process indicators, simple operation, and no introduction of hazards. It provides a reference for the processing technology of phosphate-processed Pinellia ternata, lays the foundation for the quality stability of phosphate-processed Pinellia ternata, and ensures the safety and efficacy of traditional Chinese medicine. Attached Figure Description

[0035] Figure 1 This is the standard curve for oxalic acid.

[0036] Figure 2 The results are for the phosphate-processed Pinellia ternata, raw Pinellia ternata, and processed Pinellia ternata in Example 5. Detailed Implementation

[0037] The present invention will be further described below with reference to embodiments. The embodiments are only used to illustrate the present invention and do not constitute a limitation on the scope of the claims. Other alternative means that can be conceived by those skilled in the art are all within the scope of the claims of the present invention.

[0038] Example 1

[0039] Take 50g of raw Pinellia ternata and place it in a sealed container. Add 125mL of 0.20mol / L sodium hexametaphosphate solution to the Pinellia ternata and soak it at room temperature (25±2℃) for 3 days. Then cut it into thick slices and dry it at 50℃ for 12 hours to obtain the processed Pinellia ternata. For every 100kg of Pinellia ternata, use 31kg of sodium hexametaphosphate.

[0040] Example 2

[0041] Take 50g of raw Pinellia ternata and place it in a sealed container. Add 125mL of a 0.20mol / L sodium tripolyphosphate / sodium pyrophosphate (molar ratio 10 / 1) composite solution to the Pinellia ternata and soak it at room temperature (25±2℃) for 3 days. Then cut it into thick slices and dry it at 50℃ for 12 hours to obtain the processed Pinellia ternata. For every 100kg of Pinellia ternata, use 19kg of sodium tripolyphosphate and sodium pyrophosphate composite salt.

[0042] Example 3

[0043] Take 50g of raw Pinellia ternata and place it in a sealed container. Add 125mL of a 0.01mol / L sodium hexametaphosphate / sodium tripolyphosphate / sodium pyrophosphate (molar ratio 30 / 1 / 5) composite solution to the Pinellia ternata. Soak at room temperature (25±2℃) for 3 days, then cut into thick slices and dry at 50℃ for 12 hours to obtain processed Pinellia ternata. For every 100kg of Pinellia ternata, use 1.5kg of a composite salt of sodium hexametaphosphate, sodium tripolyphosphate, and sodium pyrophosphate.

[0044] Example 4

[0045] Take 50g of raw Pinellia ternata and place it in a sealed container. Add 125mL of a 0.25mol / L sodium hexametaphosphate / sodium tripolyphosphate / sodium pyrophosphate (molar ratio 30 / 1 / 5) composite solution to the Pinellia ternata. Soak at 60℃ for 3 days, then cut into thick slices and dry at 50℃ for 12 hours to obtain processed Pinellia ternata. For every 100kg of Pinellia ternata, use 36kg of a composite salt of sodium hexametaphosphate, sodium tripolyphosphate, and sodium pyrophosphate.

[0046] Example 5

[0047] Take 50g of raw Pinellia ternata and place it in a sealed container. Add 175mL of a 0.30mol / L sodium hexametaphosphate / sodium tripolyphosphate / sodium pyrophosphate (molar ratio 30 / 1 / 5) composite solution to the Pinellia ternata. Soak at room temperature (25±2℃) for 4 days, then cut into thick slices and dry at 50℃ for 12 hours to obtain processed Pinellia ternata. For every 100kg of Pinellia ternata, use 61kg of a composite salt of sodium hexametaphosphate, sodium tripolyphosphate, and sodium pyrophosphate.

[0048] Example 6

[0049] Take 50g of raw Pinellia ternata and place it in a sealed container. Add 125mL of a 0.20mol / L sodium hexametaphosphate, sodium tripolyphosphate, and sodium pyrophosphate (molar ratio 30 / 1 / 5) compound solution to the Pinellia ternata. Soak at room temperature (25±2℃) for 24 hours until there is no white core inside. Then boil at 100℃ for 3 hours, and then cut into thick slices and dry at 50℃ for 12 hours to obtain the processed Pinellia ternata. For every 100kg of Pinellia ternata, use 29kg of the sodium hexametaphosphate, sodium tripolyphosphate, and sodium pyrophosphate compound salt.

[0050] Comparative Example 1

[0051] Raw Pinellia ternata group: Except for the absence of phosphate solution, the processing method was the same as in Example 1; Processed Pinellia ternata group: Processed according to the method in the 2020 edition of the Chinese Pharmacopoeia. The products produced according to the processes in Examples 1-6, the raw Pinellia ternata group, and the processed Pinellia ternata group were all tested according to the detection method in Example 7.

[0052] Example 7

[0053] (a) The method for determining the content of calcium oxalate needle crystals includes the following steps:

[0054] 1) Chromatographic conditions

[0055] The chromatographic column was SinoPak SP AQ-C18 (250 mm × 4.6 mm, 5 μm), the mobile phase was 0.5% (v / v) phosphoric acid-water, the injection volume was 10 μL, the column temperature was 28℃, the flow rate was 1.0 ml / min, and the detection wavelength was 220 nm.

[0056] 2) Preparation of reference solution

[0057] Accurately weigh 21.18 mg of oxalic acid reference standard, place it in a 10 mL volumetric flask, and dilute to the mark with water to prepare a 1 mL stock solution containing 2.118 mg of the reference standard.

[0058] 3) Preparation of the test solution

[0059] Accurately weigh approximately 0.2 g of Pinellia ternata sample powder (passed through a 60-mesh sieve), place it in a centrifuge tube, add 3 mL of ultrapure water and mix well. Heat in a 60°C water bath for 20 min, centrifuge and discard the supernatant. Repeat the above operation once. Add 0.4 mL of hydrochloric acid solution (volume ratio 1:1) and 3.0 mL of ultrapure water to the residue, mix well, heat in a 60°C water bath for 30 min, centrifuge and collect the supernatant. Place it in a 5 mL volumetric flask and dilute to the mark to obtain the test solution. Filter through a 0.22 μm microporous membrane for later use.

[0060] 4) Plotting the standard curve

[0061] Accurately pipette an appropriate amount of the oxalic acid reference standard stock solution prepared in step 2), and dilute it with water to prepare a series of solutions with concentrations of 10.59 μg / mL, 52.95 μg / mL, 105.90 μg / mL, 158.85 μg / mL, 211.80 μg / mL, and 264.75 μg / mL. Inject these solutions according to the HPLC chromatographic conditions in step 1). Plot a standard curve with concentration (μg / mL) on the x-axis (X) and peak area (mAU*min) on the y-axis (e.g., oxalic acid standard curve). Figure 1 (As shown).

[0062] (II) The method for determining fingerprint similarity includes the following steps:

[0063] 1) Chromatographic conditions

[0064] The chromatographic column was SinoPak SP AQ-C18 (250 mm × 4.6 mm, 5 μm), the mobile phase was acetonitrile-0.1% (v / v) formic acid-water, the injection volume was 10 μL, the column temperature was 30℃, the flow rate was 1.0 ml / min, the detection wavelength was 260 nm, and the gradient elution program was as follows;

[0065] Table 1 shows the gradient elution procedure.

[0066]

[0067]

[0068] 2) Preparation of the test solution

[0069] Accurately weigh 1.0g of Pinellia ternata powder (passed through a 60-mesh sieve), place it in an Erlenmeyer flask, add 20ml of 50% (v / v) methanol, seal tightly, soak for 30min, sonicate for 1h, filter, take 15ml of the filtrate, evaporate to dryness, add water to make up to 2ml in a volumetric flask, shake well, and filter through a 0.22μm microporous membrane to obtain the final product.

[0070] Since lower calcium oxalate needle crystal content is better, the calcium oxalate needle crystal content was reverse-engineered to ensure the result was within the range [0,1]. The comprehensive score was calculated as: calcium oxalate needle crystal content * 50 + fingerprint spectrum similarity * 50. The comprehensive evaluation results of phosphate-processed Pinellia ternata are shown in Table 2.

[0071] Table 2 shows the comprehensive evaluation results of phosphate-processed Pinellia ternata.

[0072]

[0073] The results showed that the processed Pinellia ternata in the examples all had reduced calcium oxalate needle crystal content and achieved better overall scores than raw Pinellia ternata. In particular, the overall scores of Examples 4, 5, and 6 exceeded the overall score of processed Pinellia ternata in the 2020 edition of the Chinese Pharmacopoeia. In summary, this invention effectively reduces the irritation of Pinellia ternata, retains its components, and avoids the use of alum, making it a significant invention.

[0074] The verification index method for the product of the phosphate-processed Pinellia ternata described in this invention is the determination of the content of lectin protein; (Yu Hongli, Xie Yuwei, Wu Hao, et al. Determination of Pinellia ternata lectin content in Pinellia ternata and its processed products by ELISA [J]. Chinese Drug Standards, 2023, 24(03):268-274. DOI:10.19778 / j.chp.2023.03.006.)

[0075] The products produced according to the process of Example 5, the raw Pinellia ternata group, and the processed Pinellia ternata group were tested according to the testing method of Example 8.

[0076] Example 8

[0077] (a) The method for determining the content of lectin protein includes the following steps:

[0078] 1) Preparation of the test solution

[0079] Take 0.25g of sample powder (passed through a 60-mesh sieve), accurately measure the concentration, add 20 times the amount of ultrapure water, shake for 2 hours, filter, take the supernatant, extract the residue twice more, combine the supernatants, and dilute to 25mL. Store at 4℃ for later use.

[0080] Sample measurement results are as follows Figure 2 As shown:

[0081] The results showed that the present invention significantly reduced the lectin protein content of Pinellia ternata. The relative content of lectin protein in the processed Pinellia ternata in Example 5 was not significantly different from that in the processed Pinellia ternata. In summary, the present invention effectively reduces the irritant toxicity of Pinellia ternata while retaining its components, and avoids the use of alum, making it a significant invention.

[0082] For those skilled in the art, the present invention is not limited to the details of the exemplary embodiments described above. The scope of the invention is defined by the appended claims rather than the foregoing description, and all variations falling within the meaning and scope of equivalents of the claims are included within the present invention. Therefore, any modifications or improvements made without departing from the spirit of the present invention are within the scope of protection claimed by the present invention.

Claims

1. A method for processing traditional Chinese medicine, characterized in that, The method includes the following steps: under sealed conditions, the raw Chinese medicinal material is processed in a phosphate solution, then cut into thick slices and dried to obtain the processed Chinese medicinal material; the Chinese medicinal material is Pinellia ternata; The processing method is as follows (1) or (2) or (3): (1) Soak the raw Chinese medicinal materials in a phosphate solution for 0.5 to 7 days at a temperature of 10 to 100℃; (2) Soak the raw Chinese medicinal materials in phosphate solution until there is no white core inside, then boil for 0.5 to 12 hours; (3) Soak the raw Chinese medicine under the conditions described in (1) and then take it out; then boil the ginger slices, phosphate solution and raw Chinese medicine together until thoroughly cooked; The phosphate is any one or a combination of at least two of sodium hexametaphosphate, sodium pyrophosphate, and sodium tripolyphosphate; When the phosphate is a combination of any two of sodium hexametaphosphate, sodium pyrophosphate, and sodium tripolyphosphate, the molar ratio is: sodium hexametaphosphate:sodium tripolyphosphate = 1:100~100:1; sodium hexametaphosphate:sodium pyrophosphate = 1:100~100:1; sodium tripolyphosphate:sodium pyrophosphate = 1:100~100:1; when the phosphate is a combination of sodium hexametaphosphate, sodium pyrophosphate, and sodium tripolyphosphate, the molar ratio is: sodium hexametaphosphate, sodium pyrophosphate, and sodium tripolyphosphate = 2~110:1~100:1~100; The concentration of the phosphate solution is 0.01~1.5 mol / L; the ratio of the raw Chinese medicinal product to the phosphate solution (g / ml) is 1:1~35.

2. The method for processing traditional Chinese medicine according to claim 1, characterized in that, When the phosphate is any combination of two of sodium hexametaphosphate, sodium pyrophosphate and sodium tripolyphosphate, the ratio of sodium hexametaphosphate to sodium tripolyphosphate is 1:10 to 10:1, based on the molar ratio. Sodium hexametaphosphate:sodium pyrophosphate = 1:10~10:1; Sodium tripolyphosphate:sodium pyrophosphate = 1:10~10:1; when the phosphate is a combination of sodium hexametaphosphate, sodium pyrophosphate and sodium tripolyphosphate, the molar ratio of sodium hexametaphosphate, sodium pyrophosphate and sodium tripolyphosphate is 30~110:5~10:

1.

3. The method for processing traditional Chinese medicine according to claim 1, characterized in that, The concentration of the phosphate solution is 0.01~0.7 mol / L.

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