Fresh cutting process of bupleurum chinense decoction pieces in production place

Abstract

The invention provides a technology for cutting bupleurum chinense medicinal material while being fresh in a producing area, and belongs to the technical field of preparation of traditional Chinese medicine decoction pieces. The process for cutting the bupleurum chinense medicinal material while being fresh in the production place comprises the following steps: pretreating bupleurum chinense freshly dug in the production place, drying for the first time until the water content is 28.2-44.9%, slicing, and drying for the second time to obtain bupleurum chinense decoction pieces. By controlling the water content of the aired bupleurum chinense in the production area, the problems that the water content of the traditional Chinese medicinal materials is too high to cause warped pieces in the cutting process, and the water content of the traditional Chinese medicinal materials is too low to cause cracking to reduce the yield are solved. All examinations of the bupleurum chinense decoction pieces prepared by the process conform to the provisions of pharmacopeia.

Description

Technical Field

[0001] The invention belongs to the technical field of preparation of Chinese herbal medicine slices, and in particular relates to a process for cutting northern bupleurum slices while they are fresh at the place of origin. Background Art

[0002] Bupleurum chinensie DC is the dried root of Bupleurum chinensie DC, a plant of the genus Bupleurum in the family Apiaceae. It has the effects of relieving fever, relieving liver depression, and raising Yang Qi. It is mainly produced in Northeast my country, North China, Northwest China and other places. Bupleurum chinensie DC is one of the famous "Qin medicines" in Shaanxi Province. The best quality is produced in Baoji in Shaanxi Province. Modern pharmacological research has proved that Bupleurum chinensie DC has antipyretic, sedative, analgesic, anti-inflammatory, antibacterial, immune-enhancing, anti-depressant and anti-tumor effects.

[0003] The traditional processing technology of Bupleurum slices is: dig the roots of Bupleurum, remove impurities and residual stems, dry them in the sun, wash them, add 50% water to moisten them for 6-8 hours until they are moist, cut them into thick slices, dry them in the sun or dry them below 80℃ to make slices. Cutting fresh Chinese medicinal materials at the origin refers to the method of processing them immediately after harvesting, cutting the cleaned fresh Chinese medicinal materials into slices, segments, blocks, petals and other shapes, and then drying them. Compared with the traditional method of cutting slices, cutting fresh eliminates the processing links such as drying and soaking of medicinal materials. After arriving at the medicinal material factory, only simple cleaning and selection are required, which reduces the production cost of Chinese medicinal slice processing enterprises and improves work efficiency. In addition, cutting fresh can also effectively avoid mildew and contamination of Chinese medicinal materials due to long drying and soaking time, avoid dissolution and loss of effective ingredients or hydrolysis and enzymolysis, avoid sulfur fumigation and insect infestation, reduce the risk of substandard quality of Chinese medicinal slices, improve their clinical efficacy, and achieve the goal of "reducing costs and increasing efficiency". At present, there are more than 60 varieties of Chinese medicinal materials whose fresh cutting technology has been studied, including Panax notoginseng, cinnamon, phellodendron, mint, barberry root, Sophora flavescens, Codonopsis pilosula, Polygonum cuspidatum, Ligusticum chuanxiong, Citrus aurantium, Areca catechu, papaya, Schizonepeta tenuifolia, Rehmannia glutinosa, Rheum palmatum, Rheum tanguticum, Fagopyrum scabra, Smilax china, Astragalus membranaceus, Alisma orientalis, Saposhnikovia divaricata, Gastrodia elata, Curcuma longa, Pueraria lobata, Sophora tonkinensis root, Linderae scutellariae, Dendrobium officinale, Paeonia suffruticosa, Corydalis yanhusuo, ginger, Rubia cordifolia, Fritillaria thunbergii, Polygonatum sibiricum, Cassia twig, Inula rugosa, White peony root, Rhizoma dioscoreae, Salvia miltiorrhiza, Angelica dahurica, Angelica sinensis, Acorus calamus, Dendrobium officinale, Ginseng, etc.

[0004] At present, there is no report on fresh-cut slices of Bupleurum chinense in the production area. Therefore, a process for fresh-cut slices of Bupleurum chinense in the production area is provided to provide a basis for the formulation of fresh-cut operation procedures and quality standards. Summary of the invention

[0005] In view of this, the object of the present invention is to provide a process for cutting northern bupleurum slices while they are fresh at the place of origin, which is simple and easy to implement, and makes the prepared northern bupleurum slices have the best comprehensive scores in appearance properties, extracts, thin layer chromatography results, and the contents of saikosaponin a and saikosaponin d.

[0006] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:

[0007] The invention provides a process for cutting northern bupleurum slices fresh at the production site, comprising: pretreating the northern bupleurum freshly dug at the production site, drying it for the first time to a water content of 28.2% to 44.9%, slicing it, and drying it for the second time to obtain the northern bupleurum slices.

[0008] Preferably, the growth period of the Bupleurum chinense is 1.5 to 2.5 years.

[0009] Preferably, the pretreatment includes: removing impurities and residual stems of Bupleurum chinense, and washing away soil.

[0010] Preferably, the first drying is drying in the sun or in an oven.

[0011] Preferably, the thickness of the drying is 5 to 10 cm, the drying temperature is 4 to 25°C, and the drying temperature is 68 to 72°C.

[0012] Preferably, the slice has a thickness of 2 to 4 mm.

[0013] Preferably, the second drying is performed to a moisture content of less than 10%.

[0014] The present invention also provides the Bupleurum chinense decoction pieces prepared by the fresh-cutting process at the above-mentioned production area.

[0015] Compared with the prior art, the present invention has the following beneficial effects:

[0016] The present invention provides a process for cutting fresh slices of Bupleurum chinense at the place of origin, comprising: pre-treating the freshly dug Bupleurum chinense at the place of origin, drying to a water content of 28.2% to 44.9%, slicing, and sun-drying to obtain the Bupleurum chinense slices. The Bupleurum chinense fresh-cutting process is to dig the root of Bupleurum chinense, remove the above-ground part, soil and other impurities, wash, dry to an appropriate water content, cut into thick slices, dry, sieve out fine residues and debris, and prepare the slices. During the cutting process, if the water content of the medicinal material is too high, it will cause the slices to warp, and if it is too low, it will cause the slices to crack, resulting in a decrease in the yield. The present invention solves the problem of "if the water content of the medicinal material is too high, it will cause the slices to warp, and if it is too low, it will cause the slices to crack, resulting in a decrease in the yield" by controlling the water content of the Bupleurum chinense dried at the place of origin. The prepared northern bupleurum slices by the above process have a light brown epidermis and a yellow-white cross section. Compared with the traditional process, the epidermis and cross section of the fresh-cut slices obtained by the cutting process provided by the present invention are slightly lighter in color, and the extract content thereof is increased by 3.70%, and there is no significant difference in moisture, total ash, and acid-insoluble ash. The fresh-cut northern bupleurum slices are simple, efficient, save manpower and cost, and reduce the production cost of Chinese medicine slice processing enterprises, and improve work efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 It is the cluster analysis category of different water content and qualified rate of slices of Radix Bupleuri Radix;

[0018] Figure 2 There are 3 batches of fresh slices of Bupleurum chinense;

[0019] Figure 3 There are 3 batches of traditional decoction pieces of Bupleurum chinense;

[0020] Figure 4 The thin layer chromatograms of fresh-cut slices and traditional slices of Bupleurum chinense (viewed under sunlight): 1. Bupleurum chinense reference material, 2. Bupleurosaponin a, 3. Bupleurosaponin d, 4. Fresh-cut slices 1 of Bupleurum chinense, 5. Fresh-cut slices 2 of Bupleurum chinense, 6. Fresh-cut slices 3 of Bupleurum chinense, 7. Traditional slices 1 of Bupleurum chinense, 8. Traditional slices 2 of Bupleurum chinense, 9. Traditional slices 3 of Bupleurum chinense;

[0021] Figure 5 The thin layer chromatograms of fresh-cut slices and traditional slices of Bupleurum chinense (viewed under 365nm ultraviolet light): 1. Bupleurum chinense reference material, 2. Bupleurosaponin a, 3. Bupleurosaponin d, 4. Fresh-cut slices 1 of Bupleurum chinense, 5. Fresh-cut slices 2 of Bupleurum chinense, 6. Fresh-cut slices 3 of Bupleurum chinense, 7. Traditional slices 1 of Bupleurum chinense, 8. Traditional slices 2 of Bupleurum chinense, 9. Traditional slices 3 of Bupleurum chinense;

[0022] Figure 6 HPLC spectrum of Bupleurum chinense sample: mixed reference of saikosaponin A and saikosaponin d;

[0023] Figure 7 This is the HPLC spectrum of Bupleurum chinense sample: Bupleurum chinense fresh-cut slices;

[0024] Figure 8 This is the HPLC spectrum of Bupleurum chinense sample: Traditional decoction pieces of Bupleurum chinense;

[0025] Fig. 9 These are photos of 28 batches of fresh-cut pieces of Bupleurum chinense, with a scale of 2.0 cm;

[0026] Fig.10 This is a thin layer chromatogram of fresh-cut slices of Bupleurum chinense (viewed under sunlight): 1. Fresh-cut slices of Bupleurum chinense X1, 2. Fresh-cut slices of Bupleurum chinense X2, 3. Fresh-cut slices of Bupleurum chinense X3, 4. Fresh-cut slices of Bupleurum chinense X4, 5. Fresh-cut slices of Bupleurum chinense X5, 6. Fresh-cut slices of Bupleurum chinense X6, 7. Fresh-cut slices of Bupleurum chinense X7, 8. Fresh-cut slices of Bupleurum chinense X8, 9. Fresh-cut slices of Bupleurum chinense X9, A, Bupleurosaponin a, B, Bupleurosaponin d, C, Bupleurum chinense reference material;

[0027] Fig.11 This is a thin layer chromatogram of fresh-cut slices of Bupleurum chinense (viewed under sunlight): 10, fresh-cut slices of Bupleurum chinense X10, 11, fresh-cut slices of Bupleurum chinense X11, 12, fresh-cut slices of Bupleurum chinense X12, 13, fresh-cut slices of Bupleurum chinense X13, 14, fresh-cut slices of Bupleurum chinense X14, 15, fresh-cut slices of Bupleurum chinense X15, 16, fresh-cut slices of Bupleurum chinense X16, 17, fresh-cut slices of Bupleurum chinense X17, 18, fresh-cut slices of Bupleurum chinense X18, A, saikosaponin a, B, saikosaponin d, C, reference medicinal material of Bupleurum chinense;

[0028] Fig.12 This is a thin layer chromatogram of fresh-cut slices of Bupleurum chinense (viewed under sunlight): 19, fresh-cut slices of Bupleurum chinense X19, 20, fresh-cut slices of Bupleurum chinense X20, 21, fresh-cut slices of Bupleurum chinense X21, 22, fresh-cut slices of Bupleurum chinense X22, 23, fresh-cut slices of Bupleurum chinense X23, 24, fresh-cut slices of Bupleurum chinense X24, 25, fresh-cut slices of Bupleurum chinense X25, 26, fresh-cut slices of Bupleurum chinense X26, 27, fresh-cut slices of Bupleurum chinense X27, 28, fresh-cut slices of Bupleurum chinense X28, A, saikosaponin a, B, saikosaponin d, C, reference medicinal material of Bupleurum chinense;

[0029] Fig.13 It is a thin layer chromatogram of fresh-cut slices of Bupleurum chinense (examined under ultraviolet light (365nm)): 1, fresh-cut slices of Bupleurum chinense X1, 2, fresh-cut slices of Bupleurum chinense X2, 3, fresh-cut slices of Bupleurum chinense X3, 4, fresh-cut slices of Bupleurum chinense X4, 5, fresh-cut slices of Bupleurum chinense X5, 6, fresh-cut slices of Bupleurum chinense X6, 7, fresh-cut slices of Bupleurum chinense X7, 8, fresh-cut slices of Bupleurum chinense X8, 9, fresh-cut slices of Bupleurum chinense X9, A, saikosaponin a, B, saikosaponin d, C, Bupleurum chinense reference medicinal material;

[0030] Fig.14It is a thin layer chromatogram of fresh-cut slices of Bupleurum chinense (examined under ultraviolet light (365nm)): 10, fresh-cut slices of Bupleurum chinense X10, 11, fresh-cut slices of Bupleurum chinense X11, 12, fresh-cut slices of Bupleurum chinense X12, 13, fresh-cut slices of Bupleurum chinense X13, 14, fresh-cut slices of Bupleurum chinense X14, 15, fresh-cut slices of Bupleurum chinense X15, 16, fresh-cut slices of Bupleurum chinense X16, 17, fresh-cut slices of Bupleurum chinense X17, 18, fresh-cut slices of Bupleurum chinense X18, A, saikosaponin a, B, saikosaponin d, C, Bupleurum chinense reference medicinal material;

[0031] Fig.15 It is a thin layer chromatogram of fresh-cut slices of Bupleurum chinense (examined under ultraviolet light (365nm)): 19, fresh-cut slices of Bupleurum chinense X19, 20, fresh-cut slices of Bupleurum chinense X20, 21, fresh-cut slices of Bupleurum chinense X21, 22, fresh-cut slices of Bupleurum chinense X22, 23, fresh-cut slices of Bupleurum chinense X23, 24, fresh-cut slices of Bupleurum chinense X24, 25, fresh-cut slices of Bupleurum chinense X25, 26, fresh-cut slices of Bupleurum chinense X26, 27, fresh-cut slices of Bupleurum chinense X27, 28, fresh-cut slices of Bupleurum chinense X28, A, saikosaponin a, B, saikosaponin d, C, Bupleurum chinense reference medicinal material;

[0032] Fig.16 These are the total content determination results of 4 specifications of saikosaponin a and saikosaponin d in 6 batches of samples. DETAILED DESCRIPTION

[0033] The invention provides a process for cutting northern bupleurum slices fresh at the production site, comprising: pretreating the northern bupleurum freshly dug at the production site, drying it for the first time to a water content of 28.2% to 44.9%, slicing it, and drying it for the second time to obtain the northern bupleurum slices.

[0034] In the present invention, the fine residues and debris are removed after the Bupleurum chinense slices are dried.

[0035] The growth period of the Bupleurum chinense described in the present invention is preferably 1.5 to 2.5 years, more preferably 2.5 years; the origin of the Bupleurum chinense is preferably Baoji City.

[0036] The pretreatment of the present invention preferably includes: removing impurities and residual stems of Bupleurum chinense, and washing away soil.

[0037] The first drying described in the present invention is airing or drying; the airing is preferably single-layer sunlight drying; the airing time is preferably from 8:00 am to 6:00 pm every day, and the airing is 1 to 2 days; the airing thickness is preferably 5 to 10 cm, more preferably 7 to 8 cm, and the airing temperature is preferably 4 to 25°C; the drying temperature is 68 to 72°C, preferably 69 to 71°C.

[0038] The thickness of the slices of the present invention is preferably 2-4 mm, and the moisture content of the slices during the first drying is preferably 28.2%-44.9%; the second drying is preferably dried to a moisture content of less than 10%; the second drying is sun drying or oven drying, and the sun drying temperature is preferably 4-25° C., and the time is preferably 3-4 days; the oven drying temperature is 68-72° C., preferably 69-71° C.; during the second drying, the thickness of the Bupleurum chinense slices is 1.2-1.8 cm, and the preferred thickness is 1.4-1.6 cm.

[0039] The present invention also provides the Bupleurum chinense decoction pieces prepared by the fresh-cutting process at the above-mentioned production area.

[0040] The technical solutions in the present invention will be described clearly and completely below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0041] In the following embodiments, unless otherwise specified, all of them are conventional methods.

[0042] Unless otherwise specified, the materials and reagents used in the following examples can be obtained from commercial sources.

[0043] The raw materials, equipment, reagents and drugs used in the embodiments of the present invention are as follows:

[0044] Raw materials: The raw materials used in the present invention are all fresh Bupleurum chinense medicinal materials produced in the current year (the growing period of the medicinal materials is 2.5 years) provided by Jiaxing Planting Professional Cooperative in Chencang District, Baoji City, and the medicinal material specimens are collected and identified as Bupleurum chinense DC., a plant of the Umbelliferae family, by researcher Guo Dong.

[0045] Experimental equipment and consumables: Agilent 1260 high performance liquid chromatograph (Agilent Technologies (China) Co., Ltd.), KR100-5-C18 high performance liquid chromatography column (Akzo Nobel, Sweden), XM-P22H stepless power regulation ultrasonic cleaning machine (power 500W, frequency 40KHz, Xiaomei Ultrasonic Instrument Kunshan Co., Ltd.), SQP analytical balance (Sartorius Scientific Instrument Beijing Co., Ltd.), Yongli Chinese medicine slicer (model DYQ401), electric constant temperature blower drying oven, high performance liquid chromatograph, electronic balance (one percent), electronic balance (one ten-thousandth), ultrasonic cleaning machine, UV transmission and reflectometer, electric constant temperature water bath.

[0046] Reagents and drugs: Bupleurum chinense reference material (batch number 120992-201509) was purchased from China Food and Drug Inspection Institutes; acetonitrile was chromatographically pure and purchased from Thermo Fisher Scientific (China) Co., Ltd.; water was Wahaha purified water; ethyl acetate, methanol, ethanol, sulfuric acid, hydrochloric acid, and ammonia water were all analytically pure.

[0047] Example 1

[0048] The origin and fresh cutting process of Bupleurum chinense slices

[0049] Remove impurities and residual stems from the freshly excavated Bupleurum chinense, wash the soil with water, and dry in a single layer under the sun (put it back indoors from 6:00 pm to 8:00 am the next day), with a drying thickness of about 5-10 cm and a temperature of 4-20° C. Use a medicine cutter to cut the dried Bupleurum chinense into 2-4 mm thick slices, pass through a Pharmacopoeia No. 1 sieve to remove fine powder, and dry it in the sun (at a temperature of 4-20° C., it can be dried in the sun for 3-4 days to make the water content less than 10%) to obtain Bupleurum chinense slices.

[0050] Example 2

[0051] The origin and fresh cutting process of Bupleurum chinense slices

[0052] Remove impurities and residual stems from the freshly excavated northern bupleurum, wash the soil with water, dry it in a dryer, put the washed bupleurum into a drying net (thickness 5-10cm) and a drying rack at a temperature of 70°C. Use a medicine cutter to cut the dried northern bupleurum into 2-4mm thick slices, pass through a pharmacopoeia No. 1 sieve to remove fine powder, and dry (the cut bupleurum slices are respectively put into a drying net (thickness 5-10cm) and a drying rack, and dried at a temperature of 70°C until the water content is less than 10%), and the northern bupleurum slices are obtained.

[0053] Example 3

[0054] This example compares the effects of Bupleurum chinense being dried to different moisture contents for the first time.

[0055] Study on the optimal moisture content of freshly cut Bupleurum

[0056] 1.1 Investigating the effects of different moisture contents on the cutting of medicinal materials

[0057] Take 9 batches of freshly excavated Bupleurum chinense, number them, remove impurities and residual stems, wash the soil with water, and air-dry them in a single layer under sunlight (put them back indoors from 6:00 p.m. to 8:00 a.m. the next day), with an air-drying thickness of about 5-10 cm and a temperature of 4-25° C. Use a medicine cutter to cut the 9 batches of Bupleurum chinense with different air-drying times and different water contents into 2-4 mm thick slices, pass through a Pharmacopoeia No. 1 sieve to remove fine powder, and dry them in the sun (at a temperature of 4-20° C., it can be dried in the sun for 3-4 days to make the water content less than 10%).

[0058] Each batch of freshly excavated Bupleurum chinense is cleaned and dried for 0, 6, 14, 16, 22, 28, 34, 38, 42, 46, 52, and 58 hours, and sliced ​​once. The number of slices is recorded as 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, and 12. When the medicinal materials are dried to a moisture content of 20% or less after being dried for different periods of time, the slices are stopped (the slices obtained by continuing to slice at this time are poor in shape, almost all of them are cut into fragments or pieces, and cannot meet the requirements of the yield rate). Slices can be made 5 times a day (once every 4-5 hours on average), 9:30 in the morning, 13:30 in the afternoon, 17:30, 23:30 in the evening, and 5:30 in the morning, 9 batches are cut each time, and each batch is cut into 100-150g. The properties of the medicinal materials are recorded while cutting. Take 5-10g of each batch of fresh-cut slices, take 4g of powder and put it into a weighing bottle, and measure the moisture content by drying method (n=2). The properties and origin information of 9 batches of medicinal materials are shown in Table 1, the water content of Bupleurum chinense at different cutting times is shown in Table 2, and the information of 12 cutting times of 9 batches of Bupleurum chinense (the average value of 9 batches of Bupleurum chinense) and medicinal properties are shown in Table 3.

[0059] Table 19 Batch of Small Trial Bupleurum Radix Information

[0060]

[0061] Table 2 Water content of Bupleurum chinense at different cutting times

[0062]

[0063]

[0064] Table 39 Batch 12 Cutting Information and Medicinal Material Properties Summary

[0065]

[0066] According to the results in Tables 2 and 3, when the fresh Bupleurum chinense is dried to a moisture content of 21.2% to 56.4%, thick slices can be cut. However, the optimal moisture content range for fresh cutting still needs to be optimized according to the appearance of the slices.

[0067] 1.2 Evaluation standards for the appearance of medicinal pieces

[0068] During the drying process, the outer skin color of fresh-cut Bupleurum slices changes from light yellow-brown to light brown, and the cross-section changes from off-white to yellow-white. Referring to the properties of Bupleurum slices in the 2020 edition of the "Chinese Pharmacopoeia" (the outer skin is dark brown or light brown, the cross-section is light yellow-white, the fiber is strong, the texture is hard, the odor is slightly fragrant, and the taste is slightly bitter), take 20g of the freshly cut slices obtained above and evaluate the appearance quality according to the following standards. In the test, whether the cross-section of Bupleurum is off-white or yellow-white; whether the appearance shape of the slices is complete, whether there are warped slices, cracked slices, and whether there are dregs or fragments. Therefore, based on the above points, the appearance properties of fresh-cut Bupleurum slices were evaluated with the qualified rate of slices as an indicator, and the slices with qualified properties were selected. The evaluation criteria are shown in Table 4. The evaluation results are shown in Table 5.

[0069] Table 4 Evaluation criteria for the appearance of freshly cut slices of Bupleurum chinense

[0070] Appearance Description evaluate Dark brown or light brown qualified Dark brown outer skin qualified Black outer skin Failure Cut surface pale yellowish white qualified Yellowish white cut surface qualified Cut surface grayish white Failure No warping or cracking qualified Very little warping and cracking qualified More warping and cracking Failure The surface is intact without slag and debris qualified The surface is complete with very little slag and debris qualified Surface defects with more slag and debris Failure The wood is intact and the epidermis is not damaged qualified The wood is intact, the epidermis is slightly damaged qualified There are cracks in the wood or the pith is detached, and the epidermis is damaged Failure

[0071] Table 5 Detailed table of qualified rates of fresh-cut slices of Radix Bupleuri

[0072]

[0073] 1.3 Optimization of process parameters

[0074] The traditional process of preparing Bupleurum slices was used as a reference (control). The traditional process is as follows: remove mud, sand, stems and leaves; wash the mud or other impurities attached to the surface of the medicinal material, spray with clean water, and moisten for 10-18 hours until the humidity inside and outside is consistent, which is conducive to cutting; cut 2-4mm thick slices with a chopping knife-type medicine cutter, put the Bupleurum slices into a drying net (thickness 5-10cm) and a drying rack, push them into a drying room and dry them at 70℃ for 8 hours until they are completely dry. The dried slices are passed through a medicine cleaner to remove the remaining dust, and the traditional process Bupleurum slices are obtained.

[0075] SPSS software was used to perform K-means cluster analysis on the moisture content and qualified rate of medicinal slices of 108 samples (9 batches of Bupleurum chinense in 1.1, each batch of samples cut 12 times) in this study. The results are shown in Figure 1 . The samples were divided into three categories, accounting for 25.00%, 46.30%, and 28.70% respectively. In the first category, the moisture content was lower than 28.2%, and the qualified rate of slices was lower than 39.7; in the second category, the moisture content was moderate (28.2%-44.9%), and the qualified rate of slices was 45.0%-66.1%; in the third category, the moisture content was high (greater than 44.9%), and the qualified rate of slices was 26.6%-50.6%. Therefore, only when the moisture content is moderate can the slicing effect be best. Therefore, the moisture range of fresh-cut Bupleurum chinense medicinal materials is 28.2%-44.9% (the moisture point of the 5th to 9th cutting, the dryness of the medicinal materials is 70% to 50%, and the drying time is 22-42h) as the fresh-cut indicator of northern Bupleurum chinense medicinal materials for pilot verification.

[0076] Example 4

[0077] 1 Pilot test of fresh processing of Bupleurum

[0078] 1.1 Cooperating unit: Shaanxi Tongchuan Xingshengde Pharmaceutical Co., Ltd.

[0079] 1.2 Equipment and Materials

[0080] Equipment: XSG-900 circulating water medicine washing machine (Hangzhou Chunjiang Pharmaceutical Machinery Co., Ltd.); DHS-20A halogen moisture meter (Shanghai Jinghai Instrument Co., Ltd.); KFHG-32Ⅱ Ourida intelligent drying machine (Anhui Ourida Electrical Technology Co., Ltd.); QJBC-200 chopping knife type medicine cutting machine (Hangzhou Chunjiang Pharmaceutical Machinery Co., Ltd.); air separator (Anhui Bozhou Machinery Equipment Factory); SE-750 high-speed crusher (Yongkang Shengxiang Electrical Co., Ltd.).

[0081] Materials: Three batches of Bupleurum chinense medicinal materials were all from Xiangong Town, Chencang District, Baoji City.

[0082] 1.3 Operation Method

[0083] Three batches of fresh roots of Bupleurum chinense DC. (i.e. Bupleurum chinense) of the Umbelliferae family were excavated from Xiangong Town, Chencang District, Baoji City (2.5 years old), with 100 kg in each batch.

[0084] The origin of the northern Bupleurum slices is to cut them while they are fresh. The operation process is as follows: remove the remaining stems and sieve out impurities such as soil; place the Bupleurum in a stainless steel tank and use a pressurized water pipe to flush out the remaining mud and dust; put the washed Bupleurum into a drying net (thickness 5-10cm) and a drying rack, and push it into the Orida intelligent dryer (drying room) for 2-3 hours (parameters: operating mode: drying temperature 70℃), and use a halogen moisture meter to measure the moisture content of the medicinal materials once every hour. After the 3rd hour of drying, the water content of the Bupleurum Radix was measured to be 34.05%, which is in the range of 28.2%-44.9% (the corresponding properties are: the surface of the medicinal material is light brown, the cross section is yellow-white, the fiber is strong, it is slightly prickly to hold, the root tip is broken when folded, and the main root is tough and not easy to break); the medicinal materials are quickly collected and weighed, and 10kg is taken out of each batch for standby use. The remaining Bupleurum Radix is ​​cut into 2-4mm thick slices by batch using a chopping knife-type medicine cutting machine, and the small sections of Bupleurum Radix greater than 6mm in length are screened out using a mesh screen with a 0.6cm aperture, and then cut again to meet the requirements; the 3 batches of cut Bupleurum Radix slices are respectively loaded into a drying net (thickness 5-10cm) and a drying rack, and pushed into a drying room for 8 hours to completely dry (parameters: operation mode: drying temperature 70℃). The dried slices are passed through an air separator to remove fine residues and debris. Weigh and calculate the average yield to be 22.2%; use polyethylene plastic bags to pack the qualified fresh-cut pieces, with a specification of 2kg / bag. Store the packaged pieces in a cool warehouse.

[0085] 1.4 Comparison of the process of making slices of Bupleurum chinense: Take three batches of dried Bupleurum chinense medicinal materials from the pilot test, remove the mud, sand, stems and leaves according to the traditional process; wash the mud or other impurities attached to the surface of the medicinal materials, spray with clean water, and moisten for 10 to 18 hours until the humidity inside and outside is consistent, which is conducive to cutting; cut 2 to 4 mm thick slices with a chopping knife-type medicine cutter, put the Bupleurum chinense slices into a drying net (thickness 5 to 10 cm) and a drying rack, push them into a drying room and bake at 70℃ for 8 to 10 hours until they are completely dry. After drying, the slices are passed through a medicine cleaner to remove the remaining dust, and the traditional Bupleurum chinense slices are obtained. Use polyethylene plastic bags to package qualified slices, with a specification of 2kg / bag.

[0086] 1.5 Inspection of pilot fresh-cut medicinal pieces and traditional medicinal pieces from the same batch

[0087] Three batches of fresh-cut medicinal slices and traditional medicinal slices were taken and inspected for properties, identification, inspection, extract, content determination, moisture, ash content, etc. according to the inspection methods under the Bupleurum chinense item of the 2020 edition of the "Chinese Pharmacopoeia".

[0088] 2.1 Properties: Freshly cut Bupleurum chinense is in irregular thick slices. The outer skin is light brown with longitudinal wrinkles and root marks. The cut surface is pale yellowish white and fibrous. It is hard. It has a slight fragrance and a slightly bitter taste. The properties are basically the same as those of traditional medicinal pieces, but the color of the skin and cross section is slightly different. The skin of traditional medicinal pieces is dark brown and the cross section is yellowish white, while the color of freshly cut medicinal pieces is lighter and can be seen. Figure 2 , Figure 3 .

[0089] 2.2 Thin layer identification: Take 0.5g of the powder of this product, add 20mL of methanol, ultrasonically treat for 10 minutes, filter, and concentrate the filtrate to 5mL as the test solution. Take 0.5g of the reference medicinal material of Bupleurum chinense (purchased from China Food and Drug Inspection Institute) and prepare the reference medicinal material solution in the same way. Take the reference substance of saikosaponin a (purchased from China Food and Drug Inspection Institute) and saikosaponin d (purchased from China Food and Drug Inspection Institute), add methanol to prepare a mixed solution containing 0.5mg of each per 1mL, as the reference solution. According to the thin layer chromatography method (General Rule 0502), take 5μL of each of the above three solutions and spot them on the same silica gel G thin layer plate, use ethyl acetate-ethanol-water (8:2:1) as the developing solvent, develop, take out, dry, spray with 2% p-dimethylaminobenzaldehyde in 40% sulfuric acid solution, heat at 60℃ until the spots are clearly colored, and inspect them under sunlight and ultraviolet light (365nm). In the chromatogram of the test sample, spots of the same color or fluorescent spots appear at the corresponding positions of the chromatogram of the reference medicinal material and the chromatogram of the reference sample. Figure 4 , the chromatographic results under UV light (365nm) are shown in Figure 5 .

[0090] 2.3 Extracts: According to the hot leaching method under the alcohol-soluble extract determination method (General Rule 2201), using 95% ethanol as the solvent, the extract content is greater than 11.0%. The extract content of fresh-cut slices is higher than that of traditional slices. The specific results are shown in Table 6.

[0091] Table 6 Determination results of alcohol-soluble extracts in fresh-cut and traditional slices

[0092]

[0093]

[0094] 2.4 Content determination: Determine according to high performance liquid chromatography (General Rule 0512).

[0095] Chromatographic conditions and system suitability test: octadecylsilane bonded silica gel is used as filler; acetonitrile is used as mobile phase A, water is used as mobile phase B, and gradient elution is performed according to the provisions in Table 7; the detection wavelength is 210 nm. The theoretical plate number calculated based on the saikosaponin a peak should not be less than 10,000.

[0096] Table 7 HPLC content determination mobile phase conditions of Bupleurum chinense

[0097] Time (minutes) Mobile phase A (%) Mobile phase B (%) 0～50 25→90 75→10 50～55 90 10

[0098] Preparation of reference solution: Take appropriate amount of saikosaponin a reference substance and saikosaponin d reference substance, weigh accurately, add methanol to make a solution containing 0.4 mg of saikosaponin a and 0.5 mg of saikosaponin d per 1 mL, shake well, and obtain.

[0099] Preparation of test solution: Take about 0.5g of the powder of this product (passed through a No. 4 sieve), weigh accurately, place in a stoppered conical flask, add 25mL of methanol solution containing 5% concentrated ammonia test solution, stopper, ultrasonically treat at 30℃ water temperature (power 200W, frequency 40kHz) for 30 minutes, filter, wash the container and the drug residue twice with 20mL of methanol, combine the washing liquid with the filtrate, and recover the solvent to dryness. Dissolve the residue in methanol, transfer to a 5mL volumetric flask, add methanol to the scale, shake well, filter, and take the filtrate to obtain.

[0100] Determination method: Accurately pipette 10 μL of reference solution and 10 μL of test solution respectively, inject into liquid chromatograph, and determine. The HPLC spectrum of fresh-cut slices of Bupleurum chinense is shown in Figure 6-8 The measurement results are shown in Table 8.

[0101] Table 8 HPLC content determination results of fresh-cut pieces and traditional pieces

[0102]

[0103] According to the requirements of the Pharmacopoeia, the content of saikosaponin A (C 42 H 68 O 13 ) and saikosaponin d(C 42 H 68 O 13 The total amount of saikosaponin A and saikosaponin D in fresh-cut pieces should not be less than 0.30%. The contents of fresh-cut pieces and traditional pieces are in line with the pharmacopoeia, but the total content of saikosaponin A and saikosaponin D in fresh-cut pieces is slightly lower than that in traditional pieces.

[0104] The reason for the decrease in the total content of saikosaponin A and saikosaponin d in fresh-cut pieces is the processing link of water rehydration of medicinal materials. According to the analysis of HPLC chromatograms, it was found that the two chromatographic peaks at 36min and 39min showed a large area change, and it was speculated that the two components were converted into saikosaponin A and saikosaponin d when the medicinal materials were rehydrated. Further study of 6 batches of northern Bupleurum medicinal materials found that the total content of saikosaponin A and saikosaponin d in steamed dry medicinal materials was basically the same as that of unsteamed dry medicinal materials in the same batch, and after 8h of rehydration, its content was consistent with that of traditional medicinal pieces. The 6 batches of northern Bupleurum dry medicinal materials were rehydrated for 8h, 16h, 24h, and 48h, respectively, and then dried, and the content was measured. It was found that the total content of saikosaponin A and saikosaponin d increased with the increase of rehydration time. It can be seen that the changes in the content of saikosaponin a and saikosaponin d during the water rehydration of northern Bupleurum are spontaneous reactions. The total content of saikosaponin A and saikosaponin d was positively correlated with the recovery time. Considering that the total content of saikosaponin A and saikosaponin d in fresh-cut slices was less different from that in the same batch of traditional slices, and the processing method could effectively reduce costs and improve product competitiveness, the fresh-cut process was selected.

[0105] 2.5 Moisture determination

[0106] The moisture content of fresh-cut slices and traditional slices of Bupleurum chinense was determined with reference to the second method (drying method) of moisture determination in 0832 of the 2020 edition of the "Chinese Pharmacopoeia". The results are shown in Table 9.

[0107] Table 9 Moisture determination results of fresh-cut and traditional slices

[0108]

[0109] According to Table 9, the moisture content of fresh-cut slices is slightly higher than that of traditional slices, and both meet the pharmacopoeia standards.

[0110] 2.6 Ash content determination

[0111] Referring to the ash determination method 2302 of the 2020 edition of the "Chinese Pharmacopoeia", the total ash content and acid-insoluble ash content of fresh-cut slices and traditional slices of Bupleurum chinense were determined. The results are shown in Table 10.

[0112] Table 10 Determination results of total ash and acid insoluble ash in fresh-cut and traditional slices

[0113]

[0114] According to Table 10, the total ash and acid-insoluble ash of fresh-cut slices are lower than those of traditional slices, and both meet the pharmacopoeia standards.

[0115] 2. Overall comparison of 73 batches of fresh-cut medicinal pieces and traditional medicinal pieces

[0116] After sorting out the above results, it was found that there was no significant difference between the fresh-cut slices and the traditional slices of the same batch in TLC identification, and no significant difference in properties, extract content, saikosaponin a (C 42 H 68 O 13 ) and saikosaponin d(C 42 H 68 O 13 ) have their own characteristics in terms of total content and other inspection items, but all meet the pharmacopoeia standards. The specific results are shown in Table 11. The pilot process was finally determined to be the best process for cutting Bupleurum while it is fresh.

[0117] Table 11 Comparison between fresh-cut and traditional medicinal pieces

[0118]

[0119] Example 5

[0120] Quality verification of fresh-cut slices of Bupleurum chinense

[0121] 1. Preparation of fresh-cut slices

[0122] Take 28 batches of fresh Radix Bupleuri Radix, 5 kg each, remove impurities, wash off soil with water, dry in the sun (thickness 5-10 cm) until the water content is within the range of 28.2%-44.9%, cut into 2-4 mm thick slices, dry completely (thickness about 1.5 cm), pass through the Pharmacopoeia No. 1 sieve to remove fine residues and debris, package, and make fresh-cut slices. Numbered as X1, X2, X3, ..., X28. The origin of the medicinal materials, drying conditions and water content information when cutting are shown in Table 12.

[0123] Table 12 Information on drying conditions and moisture content of medicinal materials during cutting

[0124]

[0125]

[0126] 2. Inspection of 28 batches of fresh-cut medicinal pieces

[0127] 28 batches of fresh-cut medicinal pieces were taken and inspected for properties, thin layer identification, extract, content determination, moisture, ash content, etc. according to the inspection methods under the Bupleurum chinense item of the 2020 edition of the "Chinese Pharmacopoeia".

[0128] The results of the trait test are shown in Fig. 9 :The fresh cut medicinal material of Bupleurum chinense is in irregular thick slices. The outer skin is light brown with longitudinal wrinkles and root marks. The cut surface is light yellowish white and fibrous. The texture is hard. The smell is slightly fragrant and the taste is slightly bitter. The properties are basically the same as those of traditional medicinal pieces, but the color of the skin and cross section is slightly different. The skin of traditional medicinal pieces is dark brown and the cross section is yellowish white, while the fresh cut medicinal pieces are lighter.

[0129] The thin layer identification method in 2.2 of Example 4 was adopted to perform thin layer identification on the fresh-cut pieces. The thin layer identification results are shown in Figure 10-15 , spots of the same color or fluorescent spots appear at the corresponding positions of the control medicinal material chromatogram and the reference substance chromatogram.

[0130] The test results of the alcohol-soluble extract of fresh-cut pieces, the total content of saikosaponin a and saikosaponin d, moisture, total ash and acid-insoluble ash are shown in Table 13.

[0131] Table 1328 Batch of fresh-cut slices of Bupleurum chinense with alcohol-soluble extracts and other five indicators

[0132]

[0133]

[0134] The above results showed that there was no significant difference in the identification of fresh-cut pieces in terms of properties and TLC, but no significant difference in terms of extract content, saikosaponin a (C 42 H 68 O 13 ) and saikosaponin d(C 42 H 68 O 13 ) and other inspection items have their own characteristics, all of which are better than the pharmacopoeia standards. The specific results are shown in Table 14.

[0135] Table 14 Summary of test results of fresh-cut medicinal pieces

[0136]

[0137] 3. Study on the difference of total content of saikosaponin a and saikosaponin d between fresh-cut and traditional pieces

[0138] Take 6 batches of dried Radix Bupleuri and the same batch of fresh-cut Radix Bupleuri slices, dried Radix Bupleuri slices after moistening for 8 hours, and traditional Radix Bupleuri slices of 4 specifications, and grind them into fine powder. HPLC content determination study was carried out according to the method in Example 3. The results are shown in Table 15. Fig.16 .

[0139] Table 15 Determination of the total content of saponin a and saikosaponin d in different Bupleurum

[0140]

[0141] From Table 15 and Fig.16 The results show that the total content of saikosaponin a and saikosaponin d in fresh-cut pieces is close to that in dry herbs, and the total content of saikosaponin a and saikosaponin d in samples dried after wetting dry herbs is close to that in traditional pieces. Therefore, it is speculated that the total content of saikosaponin a and saikosaponin d is related to the rewetting of dry herbs.

[0142] In summary, during the cutting process of Bupleurum chinense, too high water content will lead to warping of slices, and too low water content will lead to cracking of slices, which will reduce the yield. All inspections of the fresh-cut slices prepared by the method provided by the present invention meet the requirements of the pharmacopoeia. Compared with the traditional slices of the same batch, there is no obvious difference in the epidermis and cross-section of the fresh-cut slices under this process, the extract content is increased by 3.70%, which is better than the traditional process slices, and the total content of saikosaponin A and saikosaponin d is reduced by 0.15%, which is slightly lower than the traditional slices. There is no obvious difference in moisture, total ash, and acid-insoluble ash. The process of cutting Bupleurum chinense while fresh is simple, efficient, saves manpower and cost, and is worthy of promotion and application.

[0143] From the test results of Example 4 and the quality standard research results of 28 batches of fresh-cut slices of Bupleurum chinense in Example 5, it can be seen that the alcohol-soluble extract is the dominant index of the fresh-cut slices of Bupleurum chinense of the present invention, which is higher than that of traditional slices. The total content of saikosaponin A and saikosaponin d is slightly lower than that of traditional slices, and it is recommended to be consistent with the pharmacopoeia.

[0144] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A process for cutting fresh slices of Radix Bupleuri at the place of origin, characterized in that: include: The freshly dug Bupleurum chinense slices are pretreated, dried for the first time to a water content of 28.2% to 44.9%, sliced, and dried for the second time to obtain the Bupleurum chinense slices.

2. The process for cutting fresh fruits at the place of origin according to claim 1, characterized in that: The growth period of the Bupleurum chinense is 1.5 to 2.5 years.

3. The process for cutting fresh fruits at the place of origin according to claim 1, characterized in that: The pretreatment comprises: removing impurities and residual stems of Bupleurum chinense and washing away soil.

4. The process for cutting fresh fruits at the place of origin according to claim 1, characterized in that: The first drying is drying in the sun or drying in the oven.

5. The process for cutting fresh fruits at the place of origin according to claim 4, characterized in that: The thickness of the drying process is 5 to 10 cm, the drying temperature is 4 to 25° C., and the drying temperature is 68 to 72° C.

6. The process for cutting fresh fruits at the place of origin according to claim 1, characterized in that: The thickness of the slice is 2 to 4 mm.

7. The process for cutting freshly harvested fruits at the place of origin according to claim 1, characterized in that: The second drying is performed to a moisture content of less than 10%.

8. The Bupleurum chinense slices prepared by the fresh-cutting process according to any one of claims 1 to 7.

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