CN110596105A - Quality standard detection method of wheat malt medicinal material - Google Patents
Quality standard detection method of wheat malt medicinal material Download PDFInfo
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- CN110596105A CN110596105A CN201910879091.3A CN201910879091A CN110596105A CN 110596105 A CN110596105 A CN 110596105A CN 201910879091 A CN201910879091 A CN 201910879091A CN 110596105 A CN110596105 A CN 110596105A
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- medicinal material
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
- G01N5/045—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder for determining moisture content
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
- G01N2021/8466—Investigation of vegetal material, e.g. leaves, plants, fruits
Abstract
The invention discloses a quality standard detection method of a wheat malt medicinal material, which comprises microscopic identification, thin-layer identification and measurement of water, total ash and extract. The invention improves the standard on the basis of the original quality standard, and can effectively control the quality of the wheat malt medicinal material and improve the quality and the safety of the medicinal material under the conditions of adding microscopic identification, thin-layer identification, water content, total ash content and leaching items.
Description
Technical Field
The invention relates to the technical field of quality standards of traditional Chinese medicinal materials, in particular to a detection method of the quality standard of wheat sprouts of the traditional Chinese medicinal materials.
Background
The use of wheat as a medicine is disclosed in the "gan mai da zao tang" from jin kui Yao L ü e, cloud from Ben Cao Bian L: wheat, the one that this person grinds into flour, is a person who eats everyday. Bayuuet, summer to precocious. One kind of spring seed, poor in quality when making noodles. The malt can be used as a medicine for treating beriberi or helping digestion, and wheat malt is used for promoting digestion, strengthening stomach, regulating middle warmer, descending qi and delactation in folks of our province. Can be used for treating dyspepsia, abdominal distention, anorexia, emesis, diarrhea, and distention of breast.
The quality standard of Chinese medicinal materials and national medicinal materials in Guizhou province (2003 edition) only contains [ characters ] to evaluate the quality of the medicinal materials, and the quality standard is imperfect, so that the deep development and utilization of the medicinal materials are limited.
Disclosure of Invention
The invention aims to provide a quality standard detection method of wheat malt, which aims to solve the problems in the prior art.
The technical scheme adopted by the invention for solving the problems is as follows:
the technical scheme adopted by the invention for solving the problems is as follows: based on the existing quality standard of traditional Chinese medicinal materials and national medicinal materials in Guizhou province (2003 edition), methods for micro-identification, thin-layer identification and determination of water, total ash content and extract of wheat malt medicinal materials are added.
Wherein, the microscopic identification is the microscopic characteristics of the powder: the powder is gray white. The single grain of starch grain is similar to round, crack or herringbone of the umbilical point, and the few grains form multiple grains.
Further, the thin layer chromatography identification steps are as follows: taking 0.5g of the product powder, adding 10ml of ethanol, performing ultrasonic treatment for 20 minutes, filtering, evaporating the filtrate to dryness, and dissolving the residue with 1ml of ethanol to obtain a test solution. Preparing 0.5g of wheat malt reference medicinal material, and preparing reference medicinal material solution by the same method. Absorbing 2 μ l of the above two solutions by thin layer chromatography (0502 of the four parts of the book of Chinese pharmacopoeia 2015), respectively dropping on the same silica gel G thin layer plate, developing with chloroform-ethyl acetate (10:1) as developing agent, taking out, air drying, spraying with 10% sulfuric acid ethanol solution, and heating at 105 deg.C until the spots are clearly developed. Inspecting under an ultraviolet lamp (365 nm). Spots of the same color appear on the chromatogram of the test solution at the positions corresponding to those on the chromatogram of the control solution.
Further, the method for measuring the moisture comprises the following steps: the water content is measured according to a second method of 0832 water content measurement general rules of four departments of the version 2015 of Chinese pharmacopoeia, which is not more than 12.0 percent;
further, the method for determining the total ash content comprises the following steps: measured according to 2302 ash content measuring method of four general rules of the year 2015 edition of Chinese pharmacopoeia, 4.0 percent is not exceeded.
Further, the extract determination method comprises the following steps: the water-soluble extract of wheat malt is measured by hot dipping method under 2201 item of general rules of the four departments of the version 2015 of Chinese pharmacopoeia with water as solvent, and is not less than 42.0%.
The invention has the beneficial effects that:
the invention improves the standard on the basis of the original quality standard, and can effectively control the quality of the wheat malt medicinal material and improve the quality and the safety of the medicinal material under the conditions of adding microscopic identification, thin-layer identification, water content, total ash content and leaching items.
Drawings
FIG. 1 is a microscopic identification picture of wheat malt;
FIG. 2 is a thin layer chromatography identification system suitability test for wheat malt; 1-3, testing a sample; 4. reference medicinal materials;
FIG. 3 shows thin-layer chromatography silica gel G plates of different brands (Qingdao sea silica gel G plate; Qingdao Dingkang silica gel G plate; C. Yantaijiang friend silica gel HSG plate, sample application amount: 2 μ L (25 ℃, 58%)); 1-3, testing a sample; 4. reference medicinal materials;
FIG. 4 shows different deployment humidities (A.RH32%; B.RH58%; C.RH72%); 1-3, testing a sample; 4. reference medicinal materials;
FIG. 5 shows the different development temperatures (A.10 ℃; B.25 ℃; C.35 ℃); 1-3, testing a sample; 4. reference medicinal materials;
FIG. 6 is a TLC chart for examining the stability of the test solution; 1. the same day; 2. standing for 1 day; 3. standing for 2 days; 4. standing for 3 days; 5. reference medicinal materials;
FIG. 7 is thin layer chromatography identification of different batches of wheat malt; 1-9, different batches of wheat malt medicinal materials (detailed information is shown in table 1); 10. and (5) comparison medicinal materials.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention.
The embodiment of the invention comprises the following steps:
the original plant and sample are obtained by germinating the fruits identified as Triticum aestivum L. by medicinal plants of the institute of pharmacy of Guizhou medical university and by Zhang Xu auxiliary professor in the department of biological and pharmacology. The malt extract information is shown in table 1. (wherein XMY01 was used as a control drug).
Table 1 sample source table
[ IDENTIFICATION ] microscopic identification method for identifying microscopic characteristics of powder
The powder is gray white. The starch grains are single grains which are round-like, crack-like or herringbone like, and a few grains form compound grains with a plurality of grains, and the result is shown in figure 1.
[ IDENTIFICATION ] thin-layer chromatography for identification
1. Chromatographic Condition and System suitability test (specificity test)
Through investigating the influence thin-layer identification factors such as different extraction methods, extraction solvents, developing agents and the like of wheat malt, the identification method of the wheat malt thin-layer chromatography is established, namely: taking 0.5g of the product powder, adding 10ml of ethanol, performing ultrasonic treatment for 20 minutes, filtering, volatilizing the filtrate, and dissolving the residue with 1ml of ethanol to obtain a test solution. Preparing 0.5g of wheat malt reference medicinal material, and preparing reference medicinal material solution by the same method. Absorbing 2 μ l of the above two solutions by thin layer chromatography (0502 of the four parts of the book of Chinese pharmacopoeia 2015), respectively dropping on the same silica gel G thin layer plate, developing with chloroform-ethyl acetate (10:1) as developing agent, taking out, air drying, spraying with 10% sulfuric acid ethanol solution, and heating at 105 deg.C until the spots are clearly developed. Inspecting under an ultraviolet lamp (365 nm). The test chromatogram showed spots of the same color at the positions corresponding to those of the control chromatogram, and the results are shown in FIG. 2.
2. Durability test
2.1 investigation of thin-layer chromatography silica gel G plates of different brands
The development effects of Qingdao marine silica gel G plate, Qingdao Dingkang silica gel G plate and Yangtai Jianyou silica gel HSG plate are respectively inspected according to the proposed thin-layer chromatography identification method, and the result is shown in figure 3.
And (4) conclusion: the three brands of silica gel G plates show that the separation degrees of Qingdao ocean and Qingdao Dingkang silica gel G plates are basically consistent, which indicates that the durability of the Qingdao ocean and Qingdao Dingkang silica gel G plates is better.
2.2 investigation of different deployment humidities
The relative humidity of the development environment adjusted with sulfuric acid of different concentrations was 32%, 58%, 72% (sulfuric acid-water adjusted relative humidity), respectively, and the development was performed at room temperature to examine the effect of different relative humidities on the development, as shown in fig. 4.
And (4) conclusion: although the bands of the chromatogram map under different humidities are clear, the Rf values are different, but the medicinal materials can still be well identified, which shows that the influence of different humidity conditions on the thin-layer chromatography result of the medicinal materials is small.
2.2.3 investigation of different deployment temperatures
The samples were developed at 10, 25, 35 ℃ and a relative humidity of 58%, respectively, and the effect of different temperatures on the development was examined, as shown in FIG. 5.
And (4) conclusion: the bands of the chromatogram map at different temperatures are clear, and the difference of the Rf values is not obvious, which indicates that the medicinal material is not greatly influenced by the temperature.
2.2.4 test article solution stability investigation
Preparing test solution by the proposed method before 3 days, 2 days, 1 day and the same day, respectively dropping on the same silica gel G plate, developing, and developing as shown in FIG. 6.
And (4) conclusion: and (3) the chromatograms of the test solution which is placed for 1-3 days after being unfolded are basically consistent, and the test solution is good in stability in 3 days.
2.2 determination of the samples
The results of the measurements on the 9 samples were obtained according to the proposed thin layer chromatography identification method and are shown in FIG. 7.
[ WATER ] moisture content is determined according to the second method of 0832 moisture determination method in the four ministry of general rules of the Chinese pharmacopoeia 2015 edition, the moisture content of the wheat malt medicinal materials of 9 batches is 9.05-10.2%, and the average value is 9.69%, so the moisture content of the product is temporarily not more than 12.0%.
[ Total Ash ] Total Ash was determined by Ash determination method according to the four-part general rule 2302 of the 2015 pharmacopoeia, the total Ash of 9 batches of wheat malt medicinal materials was 2.39% -3.02%, the average value was 2.76%, and the total Ash of the product was tentatively determined to be not more than 4.0%.
[ EXTRACT ] extract is subjected to hot dipping method according to water-soluble extract determination method in 2201 extract determination method in accordance with the general rules of the four ministry of the 2015 edition of Chinese pharmacopoeia, and extract determination is carried out by using water as solvent, wherein the filtration step is changed into suction filtration. The water-soluble extract of wheat malt of 9 batches is 45.11-60.65%, the average value is 53.88%, and the water-soluble extract of the temporary product is not less than 42.0%.
TABLE 2 determination of wheat malt extract water, ash and extract
The revised standard is as follows
[ PRODUCT ] the product is a mature fruit of Triticum aestivum L. of Gramineae, and is obtained by germination. Soaking wheat grains in water, germinating at proper temperature to 5mm, and drying quickly.
[ PROPERTIES ] the product is spindle-shaped, 5-7 mm long and 3-4 mm in diameter. The surface is light yellow, the back is round, and is slightly shriveled, the center of the abdomen surface is provided with a deep-sunk longitudinal groove, the top end is blunt, and white and soft hair is provided. The embryo and fibrous root grow from the radicle of the base. The embryo bud is needle-shaped, yellow green, and about 5mm long. The fiber has a plurality of strands, and is slender and bent. Hard, white cross section and powdery. No bad smell, slightly sweet taste.
[ IDENTIFICATION ] the product is in the form of offwhite powder. The single grain of starch grain is similar to round, crack or herringbone of the umbilical point, and the few grains form multiple grains.
(2) Taking 0.5g of the product powder, adding 10ml of ethanol, performing ultrasonic treatment for 20 minutes, filtering, evaporating the filtrate to dryness, and dissolving the residue with 1ml of ethanol to obtain a test solution. Preparing 0.5g of wheat malt reference medicinal material, and preparing reference medicinal material solution by the same method. Absorbing 2 μ l of the above two solutions by thin layer chromatography (0502 of the four parts of the book of Chinese pharmacopoeia 2015), respectively dropping on the same silica gel G thin layer plate, developing with chloroform-ethyl acetate (10:1) as developing agent, taking out, air drying, spraying with 10% sulfuric acid ethanol solution, and heating at 105 deg.C until the spots are clearly developed. Inspecting under an ultraviolet lamp (365 nm). Spots of the same color appear on the chromatogram of the test solution at the positions corresponding to those on the chromatogram of the reference solution
[ EXAMINATION ] the water content should not exceed 12.0% (0832 second method in the fourth division of the design reside in the pharmacopoeia of China 2015).
The total ash content is not more than 4.0% (the general rule 2302 in the four departments of the 2015 edition in China pharmacopoeia).
[ EXTRACT ] is measured by hot dipping method under water soluble extract measuring method (2201 in the four ministry of the pharmacopoeia of China 2015 edition), and should not be less than 42.0%.
[ PROPERTIES AND FLAVOUR GUIDING CHANNEL ] is sweet and cool. It enters spleen and stomach meridians.
[ FUNCTIONS AND INDICATIONS ] can promote digestion, invigorate stomach, regulate the middle warmer, control qi downward, and promote lactation. Can be used for treating dyspepsia, abdominal distention, anorexia, emesis, diarrhea, and distention of breast.
(usage and dosage) 9-15 g; 60g is used for delactation and stir-frying.
[ STORAGE ] is placed in a ventilated and dry place to prevent moth.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the invention can be made, and equivalents and modifications of some features of the invention can be made without departing from the spirit and scope of the invention.
Claims (3)
1. A quality standard detection method of wheat malt medicinal materials is characterized by comprising the following steps: comprises microscopic identification, thin-layer identification, water content, total ash content and extract measurement.
2. The method for detecting the quality standard of the wheat malt medicinal material according to claim 1, wherein the method comprises the following steps: the thin-layer chromatography identification steps are as follows: taking the powder, adding ethanol, performing ultrasonic treatment, filtering, evaporating filtrate, dissolving residue with ethanol to obtain sample solution; preparing wheat malt reference medicinal material, and preparing reference medicinal material solution by the same method; sucking the above two solutions by thin layer chromatography, respectively dropping on the same silica gel G thin layer plate, developing with chloroform-ethyl acetate at ratio of 10:1 as developing agent, taking out, air drying, spraying 10% sulphuric acid ethanol solution, and heating at 105 deg.C until the spots are clearly developed; placing under an ultraviolet lamp for inspection; spots of the same color appear on the chromatogram of the test solution at the positions corresponding to those on the chromatogram of the control solution.
3. The method for detecting the quality standard of the wheat malt medicinal material according to claim 1, wherein the method comprises the following steps: the extract is measured by hot dipping method, and water is used as solvent to measure water soluble extract of wheat malt medicinal material, which is not less than 42.0%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113933444A (en) * | 2021-10-27 | 2022-01-14 | 国药集团同济堂（贵州）制药有限公司 | Quality detection method of elm twigs |
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