CN111983060B - Quality control method of wild six-cereal medicinal material - Google Patents
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Abstract
The invention discloses a quality control method of a wild six-cereal medicinal material, which mainly comprises the steps of measuring the content of coixol, extracting the wild six-cereal medicinal material by adopting methanol ultrasonic, performing gradient elution by taking acetonitrile as a mobile phase A and 0.1% phosphoric acid solution as a mobile phase B, and detecting the detection wavelength to be 232nm. Experiments show that the method has strong specificity and good reproducibility, and as a result, the peak time of a target peak is shortened, and the efficiency is improved. Accordingly, the inventor further researches the thin-layer identification and microscopic identification of the wild six-cereal medicinal material, and provides scientific basis for preparing scientific quality standards of the wild six-cereal medicinal material. In conclusion, the method can be used for identifying authenticity of the wild six-cereal medicinal material and evaluating quality of the wild six-cereal medicinal material, controlling quality of the wild six-cereal medicinal material and ensuring safety and effectiveness of medication for masses.
Description
Technical Field
The invention belongs to the technical field of quality control of Chinese herbal medicine materials, and particularly relates to a quality control method of wild six-cereal medicine materials.
Background
The wild six-cereal is the dry root of Coix Lacryma-jobi L. Coix lacryma-jobi, yao nationality, is called wild six cereals, also called doodles. The wild Liu cereal uses root as medicinal part, and starts from the book of its own, commonly known as the bowl root, and records in the minority nationalities such as Zhuang nationality, yao nationality and Dai nationality, and the like, and has been recorded in local medicinal material standards of the local province of China, such as the "Yunnan province Chinese medicinal material standard (2005 edition) (third album and Dai nationality medicine)" and the "Shanghai city Chinese medicinal material standard", and the like. In addition, large-scale books such as "Chinese herbal Zhi", "Chinese Daku dictionary", "Chinese herbal Association", "Chinese Ben Cao", "Guangxi Ben Cao Ji" are also briefly described for their medical value, original plant, geographical distribution and sales. The wild Liu Gu is distributed in Guangxi Yao nationality, such as Jin Xiu, may you be city, ba Ma He Fengshan and so on. It is usually grown on wet house sides, valleys, wild or cultivated. The wild Liu Gu is a common medicinal material used in the folk habit of Guangxi Yao nationality, and is widely used in Yao nationality, and is sold in part of medicine markets in Yao nationality areas, for example, the wild Liu Gu is recorded in medicinal plant resources of Yao nationality end-of-the-day medicine market in Guangxi May City. The Chinese Yao medicine records that the product has the effects of strengthening spleen, benefiting lung, clearing heat, promoting diuresis, dispelling pathogenic wind, removing dampness, and expelling parasites, and is mainly used for treating urinary tract infection or calculus, jaundice hepatitis, liver cirrhosis ascites, edema, turbid urine, leucorrhea, amenorrhea, hernia, abdominal pain due to insect accumulation, infantile pneumonia, high fever asthma and cough, rheumarthritis, nephritis and lumbago, nyctalopia, hematuria, etc.
The wild Liu Gu is mainly used as a root in Guangxi Yao nationality. The product can be picked and dug all the year round. Most of the production area is processed to remove the reed heads and the silt and dried in the sun. The literature reports that the wild six-cereal mainly contains phenols, coix seed polysaccharides, lipids (coix seed extract) and other components, and has certain pharmacological effects, wherein the coix seed extract is the main active ingredient of the wild six-cereal and has the effects of resisting cancer, easing pain, diminishing inflammation and the like. Yao medicine considers that the wild six cereals have the effects of clearing heat and promoting diuresis, strengthening spleen and killing parasites, and are used for treating heat stranguria, blood stranguria, urolithiasis, jaundice, edema, leukorrhagia, beriberi, rheumatalgia, ascariasis and other symptoms. Research data show that the benzoxanzenoid compound, coix seed extract, has the functions of resisting inflammation and relieving pain, and can inhibit histamine release of canavanine A, stimulating and immunity protein E (reactive element) sensitized mouse mast cells. In addition, researches show that coixol has an inhibitory effect on cancer cells and has a sedative and analgesic effect on the central nervous system; can effectively relieve pain and inflammatory reaction, and has antithrombotic effect; has muscle contraction effect, and has tranquilizing, analgesic, cooling and antipyretic effects on central nervous system.
The clinical curative effect of the wild six-cereal in folk is approved, but the wild six-cereal is not established as a quality control method as a common medicinal material in Guangxi Yao nationality, is difficult to control the medicinal material quality, and is unfavorable for the production, circulation, use, inspection and supervision of the wild six-cereal medicinal material. Therefore, a quality control method of the wild six-cereal is required to be established so as to control the quality of the wild six-cereal medicinal material. At present, no report on related researches of microscopic identification and thin-layer identification of wild six-cereal medicinal materials is found. Although the method for measuring the content of the wild hexa Gu Yiyi element has been reported in the literature, the mobile phase adopted in the literature method is acetonitrile-water or acetonitrile 0.1% phosphoric acid solution, and isocratic elution is adopted, so that the peak emergence time of a target peak is longer.
Disclosure of Invention
The invention aims to provide a quality control method of wild six-cereal medicinal materials, so as to identify the authenticity of the wild six-cereal medicinal materials, evaluate the quality of the wild six-cereal medicinal materials and ensure the medication safety.
In order to solve the technical problems, the invention adopts the following technical scheme:
the quality control method of the wild six-cereal medicinal material mainly comprises the steps of measuring the content of coixol, extracting the wild six-cereal medicinal material by methanol ultrasonic in the content measurement, performing gradient elution by taking acetonitrile as a mobile phase A and 0.1% phosphoric acid solution as a mobile phase B, and detecting the detection wavelength to be 232nm.
The content measurement is carried out according to the following operation: octadecylsilane chemically bonded silica is used as a filler; gradient elution is carried out according to the specification in the gradient elution program of the table;
TABLE 1 gradient elution procedure
Wherein the column temperature is 25 ℃; respectively precisely sucking 10 μl of the reference solution and the sample solution, and injecting into a liquid chromatograph for measurement.
The control solution and the test solution were prepared as follows:
control solution: precisely weighing Coicis semen reference substance, and adding methanol to obtain solution containing Coicis semen 55 μg per 1 ml;
test solution: taking 1g of wild six-cereal medicinal material powder, precisely weighing, placing into a conical flask, precisely adding 20ml of methanol, sealing, weighing, performing ultrasonic treatment for 45 minutes, cooling, weighing again, supplementing the reduced weight with methanol, shaking, filtering, and collecting subsequent filtrate.
The quality control method of the wild six-cereal medicinal material also comprises thin layer identification, wherein the thin layer identification adopts silica gel GF 254 The thin layer plate uses petroleum ether-dichloromethane-methanol-glacial acetic acid solution as developing agent.
The volume ratio of the developing agent is 6:4:1: petroleum ether-dichloromethane-methanol-glacial acetic acid solution of 0.1.
The thin layer authentication is performed as follows: sucking 4-8 μl of each of the sample solution and the control medicinal solution, and dispensing 4 μl of the control solution onto the same silica gel GF 254 And (3) unfolding the thin layer plate by using a developing agent, taking out, airing, and inspecting under an ultraviolet lamp.
The test solution, the control medicinal material solution and the control solution are prepared according to the following operations:
test solution or control medicinal material solution: collecting wild six cereal powder or wild six cereal control powder 1g, adding methanol 25ml, ultrasonic treating for 30 min, filtering, evaporating filtrate, and dissolving residue with methanol 1 ml;
control solution: taking coixol reference substance, adding methanol to make into solution containing coixol 1mg per 1 ml.
The quality control method of the wild six-cereal medicinal material also comprises microscopic identification of medicinal materials, in the microscopic identification,
epidermal cells of root cross section column 1, fang Yuanxing; the cortex is wide, 4-6 rows of hypodermis cells are round or polygonal, 1-2 rows of fibers are annularly distributed among the hypodermis cells, the fiber wall is thin and lignified, 18-20 petal-shaped cracks are formed between the hypodermis and the center column to encircle the hypodermis, and 1-3 rows of thin-wall cells are separated among the cracks; the endothelial layer is evident and the inward cell wall is obviously thickened; phloem is thin, and cells are round or irregular; the xylem is slightly wider, the 1 rows of the guide pipes are arranged in a ring along the tangential direction, and the diameter is 45-115 mu m; the medulla accounts for about one fourth of the stem, the cells are round, and the walls are thicker; the parenchyma cells contain starch grains;
the medicinal powder is gray yellow; the fiber is bundled or separated, the front end is round or broken, the fiber wall is not uniform, and round or herringbone holes are densely distributed on the fiber; the diameter of the fiber is 15-38 mu m; the starch grains are single grains or compound grains, round, semicircular or quasi-round, navel point-shaped, crack-shaped or herringbone, and the diameter is 6-16 mu m; the guide pipes are reticulate pattern guide pipes and guide pipes with edge pattern holes, and the diameters of the guide pipes are 20-68 mu m; the wood thin-wall cell is rectangular, has more dot-shaped pits, and has the length of 90-170 mu m and the width of 16-38 mu m.
Aiming at the problem that the existing wild six-cereal medicinal material lacks relevant quality standard, based on the prior art means, through research of a scientific system, the inventor establishes a quality control method of the wild six-cereal medicinal material, which mainly comprises the steps of measuring the content of coixol, extracting the wild six-cereal medicinal material by adopting methanol ultrasound, performing gradient elution by taking acetonitrile as a mobile phase A and 0.1% phosphoric acid solution as a mobile phase B, and detecting the detection wavelength to be 232nm. Experiments show that the method has strong specificity and good reproducibility, and as a result, the peak time of a target peak is shortened, and the efficiency is improved. Accordingly, the inventor further researches the thin-layer identification and microscopic identification of the wild six-cereal medicinal material, and provides scientific basis for preparing scientific quality standards of the wild six-cereal medicinal material. In conclusion, the method can be used for identifying authenticity of the wild six-cereal medicinal material and evaluating quality of the wild six-cereal medicinal material, controlling quality of the wild six-cereal medicinal material and ensuring safety and effectiveness of medication for masses.
Drawings
FIG. 1 is a view showing a structure of a cross section of a wild six-valley, in which: 1. epidermis, 2, fiber, 3, cortex, 4, fissure, 5, endothelial layer, 6, phloem, 7, xylem, 8, duct, 9, medulla.
Fig. 2 is a structural diagram of a wild six-cereal powder, in which: 1 catheter, 2 starch grains, 3 fibers, 4 wood parenchyma cells.
Fig. 3 is a thin layer identification chart of 10 different producing areas, six valleys, in which: 1-10 are wild six-cereal medicinal materials in different producing areas of 1# to 10# respectively, wherein 8# is a wild six-cereal control medicinal material; 11. a coixol reference; the characteristic spots a, b, c are dark spots.
Fig. 4 is an HPLC chromatogram, wherein: A. reference substance, b test substance, c negative control, —coix peak.
Detailed Description
The wild six cereal herbs used in the following examples are from 10 different producing areas and are identified by an expert as roots of the grass family Coix Lacryma-jobi l. The detailed information of the sources of the medicinal materials is shown in Table 2.
TABLE 2 wild six cereal numbering at different producing areas
Example 1 microscopic authentication (FIGS. 1, 2)
The microstructure of the wild six cereal herbs from 10 different producing areas was identified, and the results are shown in fig. 1:
the root cross section of the wild six cereals is 1 row, square and round. The cortex is wide, the hypodermis cells are 4-6 rows, the cells are round or polygonal, 1-2 rows of fibers are annularly distributed among the cells, the fiber wall is thin and lignified, 18-20 petal-shaped cracks are arranged between the hypodermis and the center column to encircle, and 1-3 rows of thin-wall cells are separated among the cracks. The endothelial layer is evident and the inward cell wall is markedly thickened. Phloem is thin, and cells are round or irregular. The xylem is slightly wider, and the lines of the guide pipes 1 are arranged into rings along the tangential direction, and the diameter is 45-115 mu m. The medulla is approximately one fourth of the stem, the cells are round and the walls are thicker. The parenchyma cells of the product contain starch grains.
Microscopic observations were made on all the wild six cereal powders, the results are shown in fig. 2:
the medicinal powder is gray yellow. The fiber is bundled or separated, the front end is round or broken, the fiber wall is not uniform, and round or herringbone holes are densely distributed on the fiber; the diameter of the fiber is 15-38 mu m. The starch grains are single grains or compound grains, round, semicircular or quasi-round, navel point-shaped, crack-shaped or herringbone, and the diameter is 6-16 mu m. The conduit is a reticulate conduit and a conduit with edge holes, and the diameter is 20-68 mu m. The wood thin-wall cell is rectangular, has more dot-shaped pits, and has the length of 90-170 mu m and the width of 16-38 mu m.
To sum up, microscopic identification of the wild six-cereal medicinal material is characterized in that: the root has wide transverse surface cortex, 1-2 rows of fiber are annularly distributed between the root and the root, 18-20 petal-shaped cracks are surrounded between the hypodermis and the center column, and 1-3 rows of thin-wall cells are separated between the cracks; the xylem catheter 1 rows are arranged in a ring along the tangential direction; the root cross section and the powder parenchyma cells contain starch grains; the powder is visible in the reticulate pattern conduit and the conduit with the edge holes.
EXAMPLE 2 thin layer chromatography
Taking a solution prepared from wild six-cereal medicinal material powder as a sample, taking 1g of medicinal material powder, adding 25ml of methanol, performing ultrasonic treatment for 30 minutes, filtering, evaporating filtrate to dryness, and adding 1ml of methanol into residues to dissolve the residues to obtain a sample solution; preparing 1g of wild six-cereal reference medicine solution by the same method; adding methanol into Coicis semen reference substance to obtain 1mg solution per 1ml, and taking as reference substance solution. According to thin layer chromatography (China pharmacopoeia 2015 edition rule 0502), sucking 4-8 μl of each of the test solution and the control solution, and respectively applying to the same silica gel GF 254 And (3) taking petroleum ether-dichloromethane-methanol-glacial acetic acid (6:4:1:0.1) as a developing agent on the thin layer plate, developing, taking out, airing, and putting under an ultraviolet lamp (254 nm) for detection.
The results of measuring 10 batches of medicinal material samples are shown in figure 3, and spots with the same color appear on the positions corresponding to the control medicinal material chromatogram and the control medicinal material chromatogram in the test sample chromatogram, which also shows that the TLC method has better repeatability.
Example 3 assay
1. Instrument and materials
LC-20AT high performance liquid chromatograph (shimadzu, with autosampler and DAD detector); KQ-3200DB type digital control ultrasonic cleaner (Kunming ultrasonic instruments Co., ltd.); XS205 parts per million electronic analytical balance (mertrel-tolidox, switzerland); master-S15 ultra pure water machine (Shanghai and Thai Co.), and the like. Coixol reference substance (Nanchang Beta Biotechnology Co., ltd., batch No. 20607-201609, purity 99.8%, for content determination); methanol and acetonitrile used for the mobile phase are chromatographic purity (German merck company), water is ultrapure water, and the rest reagents are all analytical purity.
2. Method of
Octadecylsilane chemically bonded silica is used as filler, and a chromatographic column is a Filman Gemini NX-C 18 (4.6 mm. Times.250 mm,5 μm); acetonitrile is taken as a mobile phase A, 0.1 percent phosphoric acid solution is taken as a mobile phase B, and gradient elution is carried out according to the rules in the gradient elution program of the table 1; the column temperature is 25 ℃, and the detection wavelength is 232nm. The theoretical plate number should be not less than 2000 calculated according to Coicis semen peak. Precisely weighing a proper amount of coixol reference substance, adding methanol to obtain a solution containing 55 μg of coixol per 1ml, and obtaining reference substance solution. About 1g of wild six-cereal medicinal material powder (sieved by a No. four sieve) is taken, precisely weighed, placed in an conical flask, precisely added with 20ml of methanol, sealed, weighed, subjected to ultrasonic treatment (with the power of 300W and the frequency of 40 KHZ) for 45 minutes, cooled, weighed again, complemented with the reduced weight by methanol, shaken uniformly, filtered, and the subsequent filtrate is taken, thus obtaining the solution of the test sample. Respectively precisely sucking 10 μl of the reference solution and the sample solution, and injecting into a liquid chromatograph for measurement.
Results: as shown in FIG. 4, the chromatogram of the sample solution and the chromatogram of the control solution have the same retention time of the chromatographic peak, whereas the chromatogram of the negative control solution has no chromatographic peak.
1> linear relationship investigation
Taking a proper amount of coixol reference substance, adding methanol to prepare a solution with the concentration of 0.184 mg/ml. Precisely sucking the above reference solutions 0.1, 1, 2, 4, 6, and 10ml respectively, placing into 10ml measuring flask, adding methanol to constant volume to 10ml respectively, and shaking. Respectively precisely sucking 10 μl of each sample solution, injecting into HPLC, taking Coicis semen peak area as ordinate, and sample injection amount (μg) as abscissa, and drawing standard curve. Obtaining a regression equation of coixol: y= 3627016.9X-38601.8, r=0.9997, and the sample injection amount of the coixol reference substance is in good linear relation with the peak area within the range of 0.0184-1.840 ug.
2> precision test
Taking the same sample solution, and continuously sampling and measuring for 6 times according to the chromatographic conditions. Results: rsd=0.30% of the area of the coix seed peak was measured 6 times. Indicating that the instrument has good precision.
3> repeatability test
6 parts of the same sample powder are taken, each part is 1g, the sample powder is precisely weighed, a sample solution is prepared, and the sample solution is measured according to the chromatographic conditions. Results: RSD of coixol content in 6 test sample solutions was 0.74%. The method is proved to have good reproducibility.
4> stability test
Taking the same sample solution, and respectively sampling and measuring at 0, 2, 4, 6, 12 and 24 hours according to the chromatographic conditions. Results: the content of coixol RSD measured 6 times is 0.01%. The method shows that the stability of the coixol in the test sample solution is good within 24 hours.
5> sample recovery test
Taking 6 parts of powder with the same sample with known content, respectively 0.5g, precisely weighing, precisely adding 20ml of coixol reference substance solution (16.00 mug/ml), preparing test sample solution, measuring coixol content according to the chromatographic condition, and calculating average recovery rate and RSD. Results: the average recovery of coixol content was determined to be 97.87%, rsd=0.02%.
3. Sample measurement
The 12 batches of medicinal material samples are measured according to the method by referring to the high performance liquid chromatography method of the general rule 0512 in the 2015 edition of Chinese pharmacopoeia, and the results are shown in Table 3.
Table 3 sample content measurement results (n=2)
The results show that: 10 batches of samples have the coix seed content of 0.0060% -0.1489% and the average content of 0.046%. According to 10 batches of samplesTaking the difference of medicinal materials sources into consideration, the standard of the product is calculated according to the dry product to contain coixol (C 8 H 7 NO 3 ) Not less than 0.010%.
Claims (2)
1. A quality control method of wild six-cereal medicinal material mainly comprises coix seed content measurement and is characterized in that: the Leymus chinensis is Coicis semen of GramineaeCoix Lacryma-jobi Dried root of L; the content measurement adopts methanol ultrasonic extraction of wild six-cereal medicinal material, acetonitrile is taken as a mobile phase A, 0.1% phosphoric acid solution is taken as a mobile phase B, gradient elution is carried out, and the detection wavelength is 232nm; the content measurement is carried out according to the following operation: octadecylsilane chemically bonded silica is used as a filler; gradient elution is carried out according to the specification in the gradient elution program of the table;
wherein the column temperature is 25 ℃; respectively precisely sucking 10 μl of the high performance liquid reference substance solution and the high performance liquid sample solution, injecting into a liquid chromatograph, and measuring to obtain; the high performance liquid sample solution is prepared as follows: taking 1g of wild six-cereal medicinal material powder, precisely weighing, placing into an conical flask, precisely adding 20ml of methanol, sealing, weighing, performing ultrasonic treatment for 45 minutes, cooling, weighing again, supplementing the reduced weight with methanol, shaking, filtering, and collecting the subsequent filtrate; the high performance liquid reference substance solution is prepared according to the following operation: precisely weighing Coicis semen reference substance, and adding methanol to obtain solution containing Coicis semen 55 μg per 1 ml;
also comprises thin layer identification, wherein the thin layer identification adopts silica gel GF 254 The thin layer plate takes petroleum ether-dichloromethane-methanol-glacial acetic acid solution as a developing agent; the volume ratio of the developing agent is 6:4:1: petroleum ether-dichloromethane-methanol-glacial acetic acid solution of 0.1;
the thin layer identification is performed as follows: sucking 4-8 μl of each thin layer identification sample solution and 4 μl of thin layer identification control medicinal material solution, and spotting on the same oneSilica gel GF 254 Spreading the thin layer plate with spreading agent, taking out, air drying, and inspecting under ultraviolet lamp;
the thin-layer identification test solution, the thin-layer identification control medicinal material solution and the thin-layer identification control solution are respectively prepared according to the following operations: thin layer identification test solution or thin layer identification control medicinal material solution: collecting wild six cereal powder or wild six cereal control powder 1g, adding methanol 25ml, ultrasonic treating for 30 min, filtering, evaporating filtrate, and dissolving residue with methanol 1 ml; thin layer identification control solution: taking coixol reference substance, adding methanol to make into solution containing coixol 1mg per 1 ml.
2. The method for controlling the quality of wild six cereal according to claim 1, further comprising microscopic identification of the medicinal material, wherein the microscopic identification includes 1 row of epidermal cells of the root cross section, fang Yuanxing; the cortex is wide, 4-6 rows of hypodermis cells are round or polygonal, 1-2 rows of fibers are annularly distributed among the hypodermis cells, the fiber wall is thin and lignified, 18-20 petal-shaped cracks are formed between the hypodermis and the middle column to encircle the hypodermis, and 1-3 rows of thin-wall cells are separated among the cracks; the endothelial layer is evident and the inward cell wall is obviously thickened; phloem is thin, and cells are round or irregular; the xylem is slightly wide, 1 row of the guide pipes are arranged in a ring along the tangential direction, and the diameter is 45-115 mu m; the medulla accounts for about one fourth of the stem, the cells are round, and the walls are thicker; the parenchyma cells contain starch grains; the medicinal powder is gray yellow; the fiber is bundled or separated, the front end is round or broken, the fiber wall is not uniform, and round or herringbone holes are densely distributed on the fiber; the diameter of the fiber is 15-38 mu m; the starch particles are single particles or compound particles, are round, semicircular or quasi-round, have navel point points, cracks or herringbone shapes, and have the diameter of 6-16 mu m; the guide pipes are reticulate pattern guide pipes and guide pipes with edge pattern holes, and the diameters of the guide pipes are 20-68 mu m; the wood parenchyma cells are rectangular, have more dot-shaped pits, and have the length of 90-170 mu m and the width of 16-38 mu m.
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| CN102552579A (en) * | 2012-01-21 | 2012-07-11 | 北京亚东生物制药有限公司 | Traditional Chinese medicine composition for treating hyperlipemia fatty liver, as well as preparation method, quality detection method and application thereof |
| CN105353053A (en) * | 2015-12-11 | 2016-02-24 | 河北中医学院 | Content determination method for scutellarin and scutellarein in sculellaria barbata medicinal material and formula granule of sculellaria barbata medicinal material |
| CN107625774A (en) * | 2017-08-30 | 2018-01-26 | 右江民族医学院 | Application and its extracting method of the cycloartenol in antineoplastic in Job's tears cauline leaf |
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| US8686031B2 (en) * | 2011-12-19 | 2014-04-01 | Joben Bio-Medical Co., Ltd. | Flavonoids and uses thereof |
| CN104173824B (en) * | 2014-07-18 | 2017-02-15 | 浙江康莱特集团有限公司 | Coix seed oil containing 8 triglycerides as well as preparation and application of coix seed oil |
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| CN102552579A (en) * | 2012-01-21 | 2012-07-11 | 北京亚东生物制药有限公司 | Traditional Chinese medicine composition for treating hyperlipemia fatty liver, as well as preparation method, quality detection method and application thereof |
| CN105353053A (en) * | 2015-12-11 | 2016-02-24 | 河北中医学院 | Content determination method for scutellarin and scutellarein in sculellaria barbata medicinal material and formula granule of sculellaria barbata medicinal material |
| CN107625774A (en) * | 2017-08-30 | 2018-01-26 | 右江民族医学院 | Application and its extracting method of the cycloartenol in antineoplastic in Job's tears cauline leaf |
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