CN112098613A - Quality detection method of wall-broken decoction pieces - Google Patents
Quality detection method of wall-broken decoction pieces Download PDFInfo
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- CN112098613A CN112098613A CN201910524848.7A CN201910524848A CN112098613A CN 112098613 A CN112098613 A CN 112098613A CN 201910524848 A CN201910524848 A CN 201910524848A CN 112098613 A CN112098613 A CN 112098613A
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- decoction pieces
- wall
- broken decoction
- test
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Abstract
The invention discloses a quality detection method of wall-broken decoction pieces, which comprises character identification and chromatographic identification; and determining the following indexes of the wall-broken decoction pieces: water, total ash, particle size distribution, limit of unbroken cells, sulfur dioxide residue, limit of microorganisms, and optional heavy metal and harmful element or pesticide residue. The invention carries out comprehensive detection on the traditional Chinese medicine wall-broken decoction pieces by adopting a mode of combining identification, inspection and optional extract measurement and content measurement, avoids the problems of counterfeiting and adulteration of the traditional Chinese medicine wall-broken decoction pieces in the production and processing process, and thus, the detection method is more objective and accurate. The detection method provided by the invention can be used for effectively controlling the quality of the traditional Chinese medicine wall-broken decoction pieces and providing an effective method for identifying the authenticity of the traditional Chinese medicine wall-broken decoction pieces.
Description
Technical Field
The invention relates to the field of quality detection of traditional Chinese medicines, in particular to a quality detection method of wall-broken decoction pieces.
Background
The traditional Chinese medicine wall-broken decoction pieces are prepared by adopting an ultramicro-pulverization technology to plant medicinal materials meeting the requirements of legal standards and breaking cell walls of the plant medicinal materials, and pulverizing the traditional Chinese medicines or the decoction pieces of the traditional Chinese medicines into powder traditional Chinese medicine decoction pieces which are directly orally taken and have the powder particle size D90 of less than or equal to 45 mu m (more than 300 meshes). Is the fourth generation of novel traditional Chinese medicine decoction pieces which are developed after the traditional Chinese medicine decoction pieces, the prescription granule decoction pieces and the single extract granules. Compared with the traditional Chinese medicine decoction pieces, the wall-broken decoction pieces take the whole components as the medicine, greatly keeps the integrity of the original components, and has the advantages of convenient taking, high dissolution rate of the effective components, high bioavailability, conservation of Chinese medicinal material resources and the like.
After the wall of the traditional Chinese medicinal materials or the traditional Chinese medicinal decoction pieces is broken, the dissolution rate of chemical components such as active ingredients and the like is changed, so that the detection methods of identification, inspection, extract measurement, content measurement and the like of the traditional Chinese medicinal decoction pieces cannot be completely applicable. In the existing quality detection methods, a complete set of quality detection method aiming at the traditional Chinese medicine wall-broken decoction pieces does not exist, the quality of the traditional Chinese medicine wall-broken decoction pieces cannot be comprehensively reflected, and the quality of the traditional Chinese medicine wall-broken decoction pieces is difficult to be effectively controlled. Therefore, a complete detection method which has a wide application range and can comprehensively reflect the quality condition of the traditional Chinese medicine wall-broken decoction pieces must be established for the traditional Chinese medicine wall-broken decoction pieces.
CN104833749A discloses a fingerprint quality detection method for chrysanthemum wall-broken decoction pieces, which covers the spectrum information of the main active ingredients of the chrysanthemum wall-broken decoction pieces, and has strong specificity and high detection speed. However, the patent does not mention other quality detection methods of the traditional Chinese medicine wall-broken decoction pieces.
CN106771010A discloses a quality standard of honeysuckle cell wall breaking powder, and the establishment of the standard increases the edible safety of the honeysuckle cell wall breaking powder. However, the particle size distribution detection method of the patent is complicated, and the authenticity of the traditional Chinese medicine wall-broken decoction pieces cannot be effectively identified.
CN102636419A discloses a method for inspecting the granularity of montmorillonite, which comprises placing a sample into a sample cylinder of a laser diffraction granularity analyzer containing water, stirring and dispersing to detect the granularity of the sample. However, the patent does not mention the quality detection method of the traditional Chinese medicine wall-broken decoction pieces.
Disclosure of Invention
In order to solve at least part of technical problems in the prior art, the invention improves the quality control of the traditional Chinese medicine wall-broken decoction pieces, and provides a detection method which is scientific, reasonable, wide in application range, good in stability and repeatability and capable of comprehensively and effectively controlling the quality of the traditional Chinese medicine wall-broken decoction pieces by adopting a method of combining identification, inspection, extract measurement and content measurement. Specifically, the present invention includes the following.
The invention provides a quality detection method of wall-broken decoction pieces, which comprises the following steps:
(1) an identification step, which comprises character identification and chromatographic identification; and
(2) the inspection step comprises the following steps of measuring the following indexes of the wall-broken decoction pieces: moisture, ash, particle size distribution, limit of unbroken cells, residual sulfur dioxide, and limit of microorganisms. Optionally, the method further comprises the measurement of residual amounts of heavy metals and harmful elements or pesticides. Preferably, the method for measuring the heavy metal and the harmful elements is selected from a heavy metal inspection method or a lead, cadmium, arsenic, mercury and copper measuring method, and the method for measuring the pesticide residue is selected from an organic chlorine pesticide residue measuring method-chromatography, an organic phosphorus pesticide residue measuring method-chromatography, a pyrethroid pesticide residue measuring method-chromatography and a pesticide multi-residue measuring method-mass spectrometry.
Preferably, in the quality detection method of the present invention, the property identification in the identification step includes taking the tested wall-broken decoction pieces at a distance of 1-10 cm2Spreading on smooth paper, flattening the surface, observing in bright place, and identifying whether the color is uniform and whether pattern color spot exists; the chromatographic identification in the identification step comprises the steps of taking the wall-broken decoction pieces to be tested, the reference medicinal materials and the reference substances, respectively dotting the wall-broken decoction pieces to be tested on the same thin-layer plate, placing the wall-broken decoction pieces in a developing container pre-saturated by a developing agent for developing, and confirming whether spots with the same color exist in the chromatogram of the wall-broken decoction pieces to be tested at the positions corresponding to the chromatogram of the reference medicinal materials and the chromatogram of the reference substances through ultraviolet lamp or sunlight inspection.
Preferably, in the quality detection method of the present invention, the thin layer plate is selected from a silica gel G thin layer plate and a silica gel GF thin layer plate254Thin layer plate, silica gel H thin layer plate, silica gel HF254At least one of a laminate sheet and a polyamide laminate sheet.
Preferably, in the quality control method of the present invention, the method for measuring moisture in step (2) is as follows:
taking 2-5 g of wall-broken decoction pieces as a test sample, flatly paving the test sample in a flat weighing bottle which is dried to constant weight, wherein the thickness is not more than 5mm, the loose test sample is not more than 10mm, precisely weighing, opening a bottle cap, drying for 5 hours at 100-105 ℃, covering the bottle cap, moving the bottle cap into a dryer, cooling for 30 minutes, precisely weighing, drying for 1 hour at the temperature, cooling, weighing until the difference between two successive weighing is not more than 5mg, and calculating the water content in percent in the test sample according to the weight loss.
Preferably, in the quality inspection method of the present invention, the method for measuring ash in step (2) includes:
taking the wall-broken decoction pieces as a test sample, placing the test sample in a crucible which is burned to constant weight, weighing the test sample, slowly heating the test sample to 500-600 ℃ until the test sample is completely carbonized, gradually raising the temperature to 500-600 ℃ so as to completely incinerate the test sample to constant weight to obtain ash, and calculating the total ash content in percent in the test sample according to the weight of residues; optionally, further comprising: and (2) adding 10ml of dilute hydrochloric acid into the ash in a crucible by a small center, covering the crucible with a surface dish, heating the crucible on a water bath for 10 minutes, flushing the surface dish with 5ml of hot water, merging washing liquor into the crucible, filtering the washing liquor by ashless filter paper, washing residues in the crucible on the filter paper by water until the washing liquor does not show chloride reaction, moving the filter residues and the filter paper into the same crucible, drying and burning the filter residues to constant weight, and calculating the content of acid-insoluble ash in percentage in the test sample according to the weight of the residues. It is noted that the ash determination method includes determination of total ash and optionally further includes determination of acid insoluble ash. If only the total ash content is measured, the amount of the test sample is 2-3 g, for example, if the acid-insoluble ash content is measured, the amount of the test sample is 3-5 g.
Preferably, in the quality inspection method of the present invention, the method of measuring the particle size distribution is as follows: taking the wall-broken decoction pieces, measuring the particle size of the powder with a laser particle size analyzer, and taking the D90 value as the index of particle size distribution, wherein the particle size distribution D90 should not be more than 45 μm.
Preferably, in the quality detection method of the present invention, the method for determining the limit of unbroken cells is as follows:
taking 0.01g of wall-broken decoction pieces, adding 0.5ml of chloral hydrate test solution and water in a ratio of 1:1, performing ultrasonic treatment until the wall-broken decoction pieces are completely dissolved, sucking all the solution and loading the solution into tablets, wherein the granules are not overflowed, have no bubbles and are uniformly distributed, and the number of the complete cells with the diameter of more than 100 mu m is not more than 100 when the tablets are inspected by a 100-fold microscope.
Preferably, in the quality inspection method of the present invention, the method for measuring the residual amount of sulfur dioxide is as follows:
taking 10g of wall-broken decoction pieces, precisely weighing, placing the wall-broken decoction pieces in a two-neck round-bottom flask, adding 300-400 ml of water, opening a reflux condenser tube to supply water, connecting a rubber air duct at an opening E at the upper end of the condenser tube to the bottom of a 100ml conical flask, adding 50ml of 3% hydrogen peroxide solution into the conical flask to serve as absorption liquid, adding 3 drops of 2.5mg/ml methyl red ethanol solution indicator into the absorption liquid before use, titrating the solution to yellow by using 0.01mol/L sodium hydroxide titration solution, introducing nitrogen, and adjusting the gas flow to 0.2L/min by using a flow meter; opening a piston of the separating funnel C, enabling 6mol/L hydrochloric acid solution to flow into a distillation flask, immediately heating the solution in the two-neck flask to boil, and keeping slight boiling; after the water in the flask is boiled for 1.5 hours, the heating is stopped, the absorption liquid is placed on a magnetic stirrer for continuous stirring after being cooled down, the titration is carried out by using 0.01mol/L sodium hydroxide titration solution until the yellow duration time is 20 seconds and the titration result is corrected by using a blank experiment.
Preferably, in the quality control method of the present invention, the method for measuring the limit of microorganisms is selected from the group consisting of a microorganism counting method and a controlled bacteria assay method. The criteria for the determination of microbial limits can be found in the regulation of pharmacopoeia 1107, 2015 edition.
Preferably, the quality detection method of the present invention further comprises (3) extract measurement and/or (4) active ingredient content measurement; wherein: the extract determination comprises water-soluble extract determination, alcohol-soluble extract determination and volatile ether extract determination; the content determination of the active ingredients comprises the following steps:
a. high performance liquid chromatography: octadecylsilane chemically bonded silica is used as a filling agent; methanol-water, acetonitrile-phosphoric acid and acetonitrile-formic acid are taken as mobile phases; at a particular detection wavelength; preparing a reference substance solution and a test solution from the reference substance and the test solution, respectively and precisely sucking the reference substance solution and the test solution, injecting the reference substance solution and the test solution into a liquid chromatograph, eluting by using a mobile phase, and measuring; or
b. Uv-vis spectrophotometry: preparing a reference substance solution and a test solution from the reference substance and the test substance; preparation of a standard curve: respectively and precisely measuring reference substance solutions with different proportions, placing the reference substance solutions in a test tube with a plug, preparing, taking a corresponding reagent as a blank, placing the prepared solution in a quartz absorption cell, measuring absorbance within the wavelength range of 190-800 nm, drawing a standard curve by taking the absorbance as a vertical coordinate and the concentration as a horizontal coordinate, precisely measuring a corresponding sample solution, performing the same operation according to the preparation method of the standard curve, measuring the absorbance, reading the content of a substance to be measured in the sample solution from the standard curve, and calculating to obtain the test substance.
According to the invention, firstly, the crushing uniformity of the traditional Chinese medicine wall-broken decoction pieces and the authenticity of the traditional Chinese medicine wall-broken decoction pieces can be effectively judged through appearance characters and smell.
In addition, the reference medicinal materials and the reference products used in the thin-layer identification are purchased from Chinese food and drug verification research institutes, so that the sources and the authenticity of the reference medicinal materials and the reference products are ensured, and an effective and reliable basis is provided for identifying the authenticity of the sample.
Further, the particle size distribution test of the present invention: the method directly uses the laser particle size analyzer to detect the particle size, has the advantages of simple operation, convenient use and quick and accurate detection, greatly saves the time for detecting the particle size in the production process of the traditional Chinese medicine wall-broken decoction pieces, can detect the particle size in time in the production process and improves the production efficiency.
In conclusion, the invention comprehensively detects the traditional Chinese medicine wall-broken decoction pieces by adopting a mode of combining identification, inspection, extract measurement and content measurement, and avoids the problems of counterfeiting and adulteration of the traditional Chinese medicine wall-broken decoction pieces in the production and processing processes, thereby enabling the detection method of the invention to be more objective and accurate. The existing detection method can only detect specific components in the traditional Chinese medicine wall-broken decoction pieces, and although the quality of the traditional Chinese medicine wall-broken decoction pieces can also be controlled, the detection method needs to be further improved. The detection method provided by the invention can be used for effectively controlling the quality of the traditional Chinese medicine wall-broken decoction pieces and providing an effective method for identifying the authenticity of the traditional Chinese medicine wall-broken decoction pieces.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that the upper and lower limits of the range, and each intervening value therebetween, is specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control. Unless otherwise indicated, "%" is percent by weight.
Example 1
In this embodiment, the quality detection method of the present invention is illustrated by taking polyporus umbellatus wall-broken decoction pieces as an example. The embodiment comprises the following steps:
1. the characteristics are as follows: spreading cell wall-broken decoction pieces of Polyporus onto smooth paper for 5cm2The surface of the polyporus umbellatus is flattened, and the polyporus umbellatus wall-broken decoction pieces are observed in a bright place and are brown to brownish black granules or powder. Light smell, light taste, uniform color and no mottle.
2. And (3) identification: taking 1g of the product powder, adding 20ml of methanol, carrying out ultrasonic treatment for 30 minutes, filtering, and taking the filtrate as a test solution. Taking ergosterol control, adding methanol to obtain solution containing 1mg per 1ml, and making into control solution. Performing thin layer chromatography test by sucking 20 μ 1 of sample solution and control solution and 4 μ l of control solution, respectively, dropping on the same silica gel G thin layer plate, developing with petroleum ether (60-90 deg.C) -ethyl acetate (3:1) as developing agent, taking out, air drying, spraying with 2% vanillin-sulfuric acid solution, and heating at 105 deg.C until the spots are clearly developed. Spots of the same color appear on the chromatogram of the test solution at the positions corresponding to those on the chromatograms of the reference medicinal material and the reference solution.
3. And (4) checking:
(1) moisture content: precisely taking 2-5 g of the product, flatly paving the product in a flat weighing bottle which is dried to constant weight, wherein the thickness is not more than 5mm, the thickness of a loose test product is not more than 10mm, precisely weighing, opening a bottle cap, drying at 105 ℃ for 5 hours, covering the bottle cap, moving the bottle cap into a dryer, cooling for 30 minutes, precisely weighing, drying at the temperature for 1 hour, cooling, weighing until the difference of two successive weighing is not more than 5 mg.
The water content (%) in the test article was calculated from the weight loss. The results are shown in Table 1:
in the formula: m isBottle (Ref. TM. bottle): weighing the bottle at constant weight; m isSample (A): the weight of the test article; m isBottle + sample: and weighing the bottle and the sample, and drying to reach the constant weight.
TABLE 1 moisture examination of polyporus umbellatus wall-broken decoction pieces
The results show that: the average water content of the wall-broken decoction pieces of Polyporus is 5.065%, and is not more than 13.0%.
(2) Total ash content: taking 3-5 g of the product, placing the product in a crucible which is burnt to constant weight, weighing the product (accurately to 0.000lg), slowly heating the product, avoiding burning, gradually raising the temperature to 500-600 ℃ until the product is completely carbonized, and completely ashing the product until the weight is constant. The total ash content (%) in the test article was calculated from the weight of the residue. The results are shown in Table 2:
in the formula, mCrucible pot: weight of constant weight crucible; m isSample (A): the weight of the test article; m isCrucible plus sample: the crucible and the sample are burned to a constant weight.
TABLE 2 Total Ash examination of cell wall-broken decoction pieces of Polyporus umbellatus
The results show that: the average ash content of the polyporus umbellatus wall-broken decoction pieces is 7.57% and is not more than 10.0%.
(3) Acid-insoluble ash: taking the ash content obtained from the total ash content, placing the ash content in a crucible, adding 10ml of dilute hydrochloric acid into the crucible by a small center, covering the crucible with a watch glass, heating the crucible in a water bath for 10min, washing the watch glass with 5ml of hot water, merging the washing liquor into the crucible, filtering the washing liquor by ashless filter paper, washing the residue in the crucible on the filter paper by water, and washing the residue until the washing liquor does not show chloride reaction. The residue was transferred to the same crucible together with the filter paper, dried, burned to a constant weight, and the acid-insoluble ash content (%) in the test sample was calculated from the weight of the residue. The results are shown in Table 3:
in the formula, mCrucible pot: weight of constant weight crucible; m is as follows: the weight of the test article; m isCrucible plus sample: the crucible and the sample are burned to a constant weight.
TABLE 3 examination of acid-insoluble ash content of wall-broken decoction pieces of Polyporus umbellatus
The results show that: the average value of the acid-insoluble ash content of the polyporus umbellatus wall-broken decoction pieces is 2.16%, and is not more than 5.0%.
(4) Particle size distribution: taking 1g, 2g and 3g of polyporus umbellatus wall-broken decoction pieces, and determining the particle size of the powder by using a BT-9300LD laser particle size analyzer, wherein the results are shown in Table 4:
TABLE 4 particle size distribution inspection of polyporus umbellatus wall-broken decoction pieces
The results show that: the average distribution value of the grain diameter D90 of the polyporus umbellatus wall-broken decoction piece sample is 31.71 mu m, and the grain diameter does not exceed 45 mu m.
(5) Cell wall broken limit is not: weighing 0.010g of the product, adding 0.5ml of chloral hydrate test solution-water (1:1), performing ultrasonic treatment until the solution is completely dissolved, sucking all the solution and loading the solution into tablets, and inspecting each tablet by a 100-fold microscope until the tablet does not overflow, has no bubbles and is uniformly distributed. The results are shown in Table 5:
TABLE 5 non-broken cell limit table for polyporus wall-broken decoction pieces
The results show that: the number average value of the particles of the 3 batches of samples of the polyporus umbellatus wall-broken decoction pieces is more than 100 microns, and the number of the particles of the intact cells is 46 but not more than 100;
(6) residual amount of sulfur dioxide: taking about 10g of the product, precisely weighing, placing the product in a two-neck round-bottom flask, adding 300-400 ml of water, connecting a scale separating funnel, introducing nitrogen to the bottom of the flask, connecting a reflux condenser pipe, connecting a rubber air duct at the E port at the upper end of the condenser pipe, placing the condenser pipe at the bottom of a 100ml conical flask, and adding 50ml of 3% hydrogen peroxide solution into the conical flask to serve as absorption liquid (the tail end of the rubber air duct is below the liquid level of the absorption liquid). Before use, 3 drops of methyl red ethanol solution indicator (2.5mg/ml) were added to the absorption solution and titrated to yellow with 0.01 mol/sodium hydroxide titrant (i.e. end point; if the end point is exceeded, the absorption solution should be discarded). Introducing nitrogen, and adjusting the gas flow to about 0.2L/min by using a flow meter; opening a piston of the split funnel C, enabling 10ml of hydrochloric acid solution (6mol/L) to flow into a distillation flask, immediately heating the solution in the two-neck flask to boil, and keeping slight boiling; after the water in the flask was boiled for 1.5 hours, the heating was stopped. After cooling, placing the absorption liquid on a magnetic stirrer for continuous stirring, titrating by using sodium hydroxide titration solution (0.01mol/L) until the yellow duration is 20 seconds and correcting the titration result by using a blank experiment; the residual amount of sulfur dioxide (mg/kg) in the test sample was calculated. The results are shown in Table 6:
in the formula: x is the total sulfur dioxide content (mg/kg) in the test article; a is the volume (ml) of the titration solution consumed by the sample; b is the volume (ml) of blank consumption titration solution; c is the concentration (mol/L) of sodium hydroxide titration solution; w is the weight (g) of the test article.
TABLE 6 examination of the residual amount of sulfur dioxide in wall-broken decoction pieces of Polyporus umbellatus
The results show that: the average value of the sulfur dioxide residue of the polyporus umbellatus wall-broken decoction pieces is 1.76mg/kg, and the sulfur dioxide residue does not exceed 150 mg/kg;
(7) the microbial limit:
10g of the product is taken for preparing the test solution, 200ml of tryptone soy peptone liquid culture medium is added, and the mixture is placed in a water bath at 40 ℃ and shaken until the mixture is completely dissolved, so that the test solution with the ratio of 1:20 is obtained.
Microbial enumeration method
Total aerobic bacteria count: 1ml of 1:20 sample solution is taken and injected into 1 plate (1 ml of each plate), and other operations are checked according to the microbial limit of non-sterile products of the four general rules 1105 in the pharmacopoeia 2015 edition of China: the plate method of microbial counting method.
Total number of mold and yeast: 1ml of 1:20 sample solution is taken and injected into 1 plate (1 ml of each plate), and other operations are checked according to the microbial limit of non-sterile products of the four general rules 1105 in the pharmacopoeia 2015 edition of China: the plate method of microbial counting method.
And (3) a controlled bacteria inspection method: 200ml of tryptone soytone liquid culture medium for salmonella, 10ml of intestinal bacterium enrichment liquid culture medium for inspecting cholate resistant gram-negative bacteria, and the microbial limit of non-sterile products is inspected according to the four general rules 1106 of Chinese pharmacopoeia 2015 edition: checking by a corresponding method specified by a control bacteria checking law.
The results show that: total aerobic bacteria number less than 104cfu/g, total number of mould and yeast less than 102cfu/g; less than 10 gram-negative bacteria resistant to bile salt4cfu/g; no salmonella is detected in every 10g of polyporus umbellatus wall-broken decoction pieces.
4. Content determination:
octadecylsilane chemically bonded silica is used as a filler in chromatographic conditions and system applicability tests; methanol is used as a mobile phase; the detection wavelength was 283 nm. The number of theoretical plates should not be less than 5000 calculated from the ergosterol peak.
Preparation of control solution an appropriate amount of ergosterol control was precisely weighed and added with methanol to make into a solution containing 50 μ g per 1 ml.
Preparing test solution by taking about 0.5g of the product, precisely weighing, placing in a conical flask with a plug, precisely adding 10ml of methanol, weighing, ultrasonically treating (power 220W, frequency 50kHz) for 1 hour, cooling, weighing again, supplementing the lost weight with methanol, shaking uniformly, filtering, and taking the subsequent filtrate.
The determination method comprises precisely sucking 20 μ l of each of the reference solution and the sample solution, injecting into liquid chromatograph, and determining. The results are shown in Table 7:
in the formula: a. theSample (A): sample peak area; a. theTo pair: average peak area of ergosterol control; cTo pair: ergosterol control concentration; wDilution factor: dilution factor in sample protocol; cWater (W): testing the moisture of the samples in the batch; l isUnit conversion: converting the unit into the same unit for calculation; mSample (A): and weighing the sample.
TABLE 7 measurement results of wall-broken decoction pieces of Polyporus umbellatus
The results show that: the average content of ergosterol in the polyporus umbellatus wall-broken decoction pieces is 0.14% and is not less than 0.050%.
Example 2
In this embodiment, the quality detection method of the present invention is illustrated by using astragalus membranaceus wall-broken decoction pieces as an example. The embodiment comprises the following steps:
1. the characteristics are as follows: taking radix astragali wall-broken decoction pieces sample, and spreading on smooth paper for 5cm2The surface of the decoction pieces is flattened, and the decoction pieces are observed in bright places, so that the astragalus membranaceus wall-broken decoction pieces are yellow white to powder. Light smell, slightly sweet taste, slightly beany flavor, uniform and consistent color and luster and no pattern and color spots.
2. And (3) identification:
(1) taking 3g of the product, adding 20ml of methanol, heating and refluxing for 1 hour, filtering, adding filtrate to a neutral alumina column (100-120 meshes, 5g, the inner diameter is 10-15 mm), eluting with 100ml of 40% methanol, collecting eluent, evaporating to dryness, dissolving residue in 30ml of water, shaking and extracting with water saturated n-butanol for 2 times, 20ml each time, combining n-butanol solutions, washing with water for 2 times, 20ml each time, discarding water solution, evaporating to dryness the n-butanol solution, and dissolving residue in 0.5ml of methanol to obtain a sample solution. And adding methanol into astragaloside IV control to obtain lmg solution per lml as control solution. Performing thin layer chromatography (general rule 0502) test, sucking 2 μ l of the above two solutions, respectively dropping on the same silica gel G thin layer plate, developing with chloroform-methanol-water (13:7:2) lower layer solution as developing agent, taking out, air drying, spraying with 10% sulphuric acid ethanol solution, and heating at 105 deg.C until the spots are clearly developed. In the chromatogram of the test solution, the same brown spots appear in the sunlight at the positions corresponding to those of the chromatogram of the control solution; the same orange-yellow fluorescent spots were shown under an ultraviolet lamp (365 nm).
(2) Taking 2g of the product, adding 30ml of ethanol, heating and refluxing for 20 minutes, filtering, evaporating the filtrate to dryness, adding 15ml of 0.3% sodium hydroxide solution into residues for dissolving, filtering, adjusting the pH value of the filtrate to 5-6 by using dilute hydrochloric acid, shaking and extracting by using 15ml of ethyl acetate, taking ethyl acetate solution, filtering by using filter paper paved with a proper amount of anhydrous sodium sulfate, and evaporating the filtrate to dryness. The residue was dissolved in ethyl acetate lml to prepare a sample solution. Preparing 2g of radix astragali control material, and preparing a control solution by the same method. Performing thin layer chromatography (general rule 0502) test, sucking the above two solutions 10 μ 1 respectively, dropping on the same silica gel G thin layer plate, developing with chloroform-methanol (10:1) as developing agent, taking out, air drying, fumigating in ammonia vapor, and inspecting under ultraviolet lamp (365 nm). The main fluorescent spots with the same color appear on the chromatogram of the test solution at the positions corresponding to the chromatograms of the reference solution.
3. And (4) checking:
(1) moisture content: taking 2-5 g of the product, paving the product in a flat weighing bottle which is dried to constant weight, wherein the thickness is not more than 5mm, the thickness of a loose test product is not more than 10mm, precisely weighing, opening a bottle cap, drying at 105 ℃ for 5 hours, covering the bottle cap, moving the bottle cap into a dryer, cooling for 30 minutes, precisely weighing, drying at the temperature for 1 hour, cooling, weighing until the difference of two successive weighing is not more than 5 mg.
The water content (%) in the test article was calculated from the weight loss. The results are shown in Table 8:
in the formula: m isBottle (Ref. TM. bottle): weighing the bottle at constant weight; m isSample (A): the weight of the test article; m isBottle + sample: and weighing the bottle and the sample, and drying to reach the constant weight.
TABLE 8 moisture examination of radix astragali wall-broken decoction pieces
The results show that: the average water content of the radix astragali wall-broken decoction pieces is 5.025% and is not more than 10.0%.
(2) Total ash content: taking 2-3 g of the product, placing the product in a crucible which is burnt to constant weight, weighing the product (accurately to 0.000lg), slowly heating the product, avoiding burning, gradually raising the temperature to 500-600 ℃ until the product is completely carbonized, and completely ashing the product until the weight is constant. The total ash content (%) in the test article was calculated from the weight of the residue. The results are shown in Table 9:
in the formula, mCrucible pot: weight of constant weight crucible; m isSample (A): the weight of the test article; m isCrucible plus sample: the crucible and the sample are burned to a constant weight.
TABLE 9 Total Ash inspection of radix astragali wall-broken decoction pieces
The results show that: the average ash content of the radix astragali wall-broken decoction pieces is 3.24%, and is not more than 5.0%.
(3) Heavy metals and harmful elements:
preparation of standard stock solution A proper amount of lead, arsenic, cadmium, mercury and copper single element standard solution is precisely measured respectively, and diluted by 10% nitric acid solution to prepare solutions with 1 mug, 0.5 mug, mug and 10 mug of lead, arsenic, cadmium, blet and copper respectively per lml.
Preparation of standard solution A proper amount of lead, arsenic, cadmium and copper standard stock solutions are precisely measured, and diluted by 10% nitric acid solution to prepare mixed solutions with a series of concentrations of 0ng, 1ng, 5ng, 10ng and 20ng of lead, 0ng, 0.5ng, 2.5ng, 5ng and l0ng of cadmium and 0ng, 50ng, 100ng, 200ng and 500ng of copper. In addition, a proper amount of mercury standard storage solution is precisely measured, and diluted by 10% nitric acid solution to prepare solutions with mercury contents of 0ng, 0.2ng, 0.5ng, 1ng, 2ng and 5ng in each lml respectively.
Preparation of internal standard solution A proper amount of germanium, indium and bismuth single element standard solution is precisely measured, and diluted by water to prepare mixed solution containing l mu g of each lml, so that the internal standard solution is obtained.
Preparation of test sample solution A test sample is dried at 60 ℃ for 2 hours, about 0.5g of the test sample is precisely weighed and placed in a pressure-resistant and high-temperature-resistant microwave digestion tank, and 5-10 ml of nitric acid is added (if the reaction is severe, the reaction is placed until the reaction stops). Sealing and digesting according to the corresponding requirements of each microwave digestion instrument and a certain digestion program. After complete digestion, cooling the digestion solution to below 60 ℃, taking out the digestion tank, cooling, transferring the digestion solution into a 50ml measuring flask, washing the digestion tank for 3 times by using a small amount of water, merging washing liquor into the measuring flask, adding 200 mu l of gold single element standard solution (1 mu g/ml), diluting with water to a scale, and shaking up to obtain the finished product (if a small amount of precipitate exists, the supernatant can be obtained by centrifugal separation if necessary).
A reagent blank solution is prepared by the same method except that the gold single element standard solution is not added.
The isotope selected in the determination by the assay is63Cu、75As、114Cd、202Hg and208pb of, wherein63Cu、75As and with72Ge is taken as an internal standard, and the internal standard,114cd is selected from115In is used as an internal standard, and the internal standard,202Hg、208pb and Pb of209Bi is used as an internal standard, and a proper correction equation is selected according to the requirements of different instruments to correct the measured elements.
An internal standard sample tube of the instrument is always inserted into an internal standard solution in the instrument analysis working process, the sample tube of the instrument is sequentially inserted into standard solutions with various concentrations for determination (the concentrations are sequentially increased), the measured value (the average value of 3 readings) is taken as a vertical coordinate, the concentration is taken as a horizontal coordinate, and a standard curve is drawn. The sample tube of the instrument is inserted into the test solution and measured, taking the average of 3 readings. The corresponding concentrations were calculated from the standard curve.
Blank experiments were performed under the same analytical conditions, with blank interferences being subtracted according to the requirements of the instrument instructions. The results are shown in Table 10:
TABLE 10 examination of heavy metals and harmful elements of radix astragali wall-broken decoction pieces
| Inspection item | Standard regulation (mg/kg) | Test results (mg/kg) |
| Lead (II) | Not more than 5mg/kg | 0.5mg/kg |
| Cadmium (Cd) | Not more than 0.3mg/kg | 0.001mg/kg |
| Arsenic (As) | Not more than 2mg/kg | 0.2mg/kg |
| Mercury | Not more than 0.2mg/kg | <0.02mg/kg |
| Copper (Cu) | Not more than 20mg/kg | 6mg/kg |
The results show that: the contents of heavy metals and harmful elements in the astragalus membranaceus wall-broken decoction pieces meet the requirements.
(4) Residual quantity of organochlorine pesticide
Chromatographic conditions and System suitability test an elastic quartz capillary column (30 m.times.0.32 mm. times.0.25 μm) using (14% -cyanopropyl-phenyl) methylpolysiloxane or (5% phenyl) methylpolysiloxane as a stationary liquid,63a Ni-ECD electron capture detector. The temperature of the sample inlet is 230 ℃, the temperature of the detector is 300 ℃, and the split-flow sample injection is not carried out. Program for programmingSequentially heating: initially 100 ℃, 10 ℃ to 220 ℃ per minute, 8 ℃ to 250 ℃ per minute, held for 10 minutes. The number of theoretical plates should not be less than 1 × 10 calculated according to the peak of alpha-BHC6The separation of two adjacent chromatographic peaks should be greater than 1.5.
Preparation of reference stock solution A proper amount of hexachloro-cyclohexane (BHC) (alpha-BHC, beta-BHC, gamma-BHC, -BHC), dichlorodiphenyl trichloroethane (DDT) (p, p '-DDE, p, p' -DDD, o, p '-DDT, p, p' -DDT) and a proper amount of a Pentachloronitrobenzene (PCNB) pesticide reference are precisely weighed and prepared into solutions containing about 4-5 mu g per 1ml by using petroleum ether (60-90 ℃) to obtain the hexachloro-cyclohexane (BHC) and the trichloronitrobenzene (PCNB) pesticide reference.
Preparation of mixed reference stock solution 0.5ml of each reference stock solution is precisely measured, placed in a 10ml measuring flask, diluted to scale with petroleum ether (60-90 ℃) and shaken up to obtain the compound.
Preparation of mixed reference solution the mixed reference stock solution is precisely measured and prepared into solutions with the concentration of 0 mug, 1 mug, 5 mug, 10 mug, 50 mug, 100 mug and 250 mug in each 1L by petroleum ether (60-90 ℃) to obtain the product.
Preparation of test sample solution about 2g of test sample is taken, precisely weighed, placed in a 100ml conical flask with a plug, added with 20ml of water and soaked overnight, precisely added with 40ml of acetone, weighed, ultrasonically treated for 30 minutes, cooled, weighed again, complemented with acetone to lose weight, added with about 6g of sodium chloride, precisely added with 30ml of dichloromethane, weighed, ultrasonically treated for 15 minutes, weighed again, complemented with dichloromethane to lose weight, placed (layered), the organic phase is rapidly transferred into a 100ml conical flask with a plug filled with a proper amount of anhydrous sodium sulfate, and placed for 4 hours. Precisely measuring 35ml, concentrating on a water bath at 40 ℃ under reduced pressure until the solution is nearly dry, adding a small amount of petroleum ether (60-90 ℃) until dichloromethane and acetone are completely removed, dissolving with the petroleum ether (60-90 ℃) and transferring to a 10ml centrifugal tube with a plug scale, precisely diluting to 5ml with the petroleum ether (60-90 ℃), carefully adding 1ml of sulfuric acid, shaking for 1 minute, centrifuging (3000 r/min) for 10 minutes, precisely measuring 2ml of supernate, placing in a concentration bottle with scale, connecting a rotary evaporator, concentrating the solution to a proper amount at 40 ℃ (or with nitrogen), and precisely diluting to 1 ml.
The measuring method precisely absorbs 1 mul of each of the test solution and the mixed reference solution with corresponding concentration, injects the test solution and the mixed reference solution into a gas chromatograph, and calculates the residual quantity of 9 organochlorine pesticides in the test solution according to an external standard method. The results are shown in Table 11:
TABLE 11 organochlorine pesticide residue inspection of radix astragali wall-broken decoction pieces
The results show that: the organochlorine pesticide residue in the astragalus membranaceus wall-broken decoction pieces meets the specification.
(5) Particle size distribution: 1g, 2g and 3g of astragalus membranaceus wall-broken decoction pieces are taken, and the particle size of the powder is measured by a BT-9300LD laser particle size analyzer, and the results are shown in Table 12:
TABLE 12 particle size distribution inspection of radix astragali broken wall decoction pieces
The results show that: the average distribution value of the particle size D90 of the astragalus membranaceus wall-broken decoction piece sample is 30.94 microns, and the particle size D90 does not exceed 45 microns.
(6) Cell wall broken limit is not: weighing 0.010g of the product, adding 0.5ml of chloral hydrate test solution-water (1:1), performing ultrasonic treatment until the solution is completely dissolved, sucking all the solution and loading the solution into tablets, and inspecting each tablet by a 100-fold microscope until the tablet does not overflow, has no bubbles and is uniformly distributed. The results are shown in Table 13:
TABLE 13 results table of broken cell limit of radix astragali
The results show that: the number average value of particles of the astragalus membranaceus wall-broken decoction pieces 3 which are larger than 100 microns and have complete cells is 80, and the number of particles is not more than 100;
(7) residual amount of sulfur dioxide: taking about 10g of the product, precisely weighing, placing the product in a two-neck round-bottom flask, adding 300-400 ml of water, connecting a scale separating funnel, introducing nitrogen to the bottom of the flask, connecting a reflux condenser pipe, connecting a rubber air duct at the E port at the upper end of the condenser pipe, placing the condenser pipe at the bottom of a 100ml conical flask, and adding 50ml of 3% hydrogen peroxide solution into the conical flask to serve as absorption liquid (the tail end of the rubber air duct is below the liquid level of the absorption liquid). Before use, 3 drops of methyl red ethanol solution indicator (2.5mg/ml) were added to the absorption solution and titrated to yellow with 0.01 mol/sodium hydroxide titrant (i.e. end point; if the end point is exceeded, the absorption solution should be discarded). Introducing nitrogen, and adjusting the gas flow to about 0.2L/min by using a flow meter; opening a piston of the split funnel C, enabling 10ml of hydrochloric acid solution (6mol/L) to flow into a distillation flask, immediately heating the solution in the two-neck flask to boil, and keeping slight boiling; after the water in the flask was boiled for 1.5 hours, the heating was stopped. After cooling, placing the absorption liquid on a magnetic stirrer for continuous stirring, titrating by using sodium hydroxide titration solution (0.01mol/L) until the yellow duration is 20 seconds and correcting the titration result by using a blank experiment; the residual amount of sulfur dioxide (mg/kg) in the test sample was calculated. The results are shown in Table 14:
in the formula: x is the total sulfur dioxide content (mg/kg) in the test article; a is the volume (ml) of the titration solution consumed by the sample; b is the volume (ml) of blank consumption titration solution; c is the concentration (mol/L) of sodium hydroxide titration solution; w is the weight (g) of the test article.
TABLE 14 checking of sulfur dioxide residue in radix astragali broken decoction pieces
The results show that: the average value of the sulfur dioxide residue of the astragalus membranaceus wall-broken decoction pieces is 4.8mg/kg and is not more than 150 mg/kg;
(8) the microbial limit:
10g of the product is taken for preparing test solution, 200ml of trypticase soy peptone liquid culture medium is added, and the mixture is placed in a water bath at 40 ℃ and shaken till being completely dissolved, namely 1:20 test solutions.
Microbial enumeration method
Total aerobic bacteria count: taking 1: 1ml of 20 test solution is poured into 1 plate (1 ml per plate), and other operations are checked according to the microbial limit of non-sterile products of the four general rules 1105 in the pharmacopoeia 2015 edition: the plate method of microbial counting method.
Total number of mold and yeast: taking 1: 1ml of 20 test solution is poured into 1 plate (1 ml per plate), and other operations are checked according to the microbial limit of non-sterile products of the four general rules 1105 in the pharmacopoeia 2015 edition: the plate method of microbial counting method.
And (3) a controlled bacteria inspection method: 200ml of tryptone soytone liquid culture medium for salmonella, 10ml of intestinal bacterium enrichment liquid culture medium for inspecting cholate resistant gram-negative bacteria, and the microbial limit of non-sterile products is inspected according to the four general rules 1106 of Chinese pharmacopoeia 2015 edition: checking by a corresponding method specified by a control bacteria checking law.
The results show that: total aerobic bacteria number less than 104cfu/g, total number of mould and yeast less than 102cfu/g; less than 10 gram-negative bacteria resistant to bile salt4cfu/g; no salmonella is detected in every 10g of polyporus umbellatus wall-broken decoction pieces.
4. Extract of plant
Taking about 4g of the product, precisely weighing, placing the product in a conical flask of 250-300 ml, precisely adding 100ml of water, sealing, cold soaking, shaking constantly within 6 hours before, standing for 18 hours, rapidly filtering by using a drying filter, precisely taking 20ml of subsequent filtrate, placing the subsequent filtrate in an evaporating dish dried to constant weight, drying the subsequent filtrate in a water bath for 3 hours at 105 ℃, cooling the subsequent filtrate in a drier for 30 minutes, and rapidly precisely weighing. The content (%) of the water-soluble extract in the test sample was calculated on a dry basis, unless otherwise specified. The results are shown in Table 15:
TABLE 15 determination results of radix astragali wall-broken decoction pieces extract
The results show that: the average value of radix astragali wall-broken decoction piece extract is 43.5%, not less than 17.0%.
5. Content determination:
(1) astragaloside IV
Octadecylsilane chemically bonded silica is used as a filler in chromatographic conditions and system applicability tests; acetonitrile-water (32:68) is used as a mobile phase; detection by an evaporative light scattering detector. The number of theoretical plates is not less than 4000 calculated according to astragaloside IV peak.
Preparation of control solution A proper amount of astragaloside IV control is precisely weighed, and methanol is added to make into solution containing 0.5mg per 1 ml.
Preparing a sample solution, precisely weighing about 4g of the product, placing the sample solution in a Soxhlet extractor, adding 40ml of methanol, cold soaking overnight, adding an appropriate amount of methanol, heating and refluxing for 4 hours, recovering a solvent from an extracting solution, concentrating to dryness, adding 10ml of water into residues, slightly heating and dissolving, shaking and extracting with water-saturated n-butyl alcohol for 4 times, 40ml each time, combining n-butyl alcohol solutions, fully washing with an ammonia test solution for 2 times, 40ml each time, discarding the ammonia solution, evaporating the n-butyl alcohol solution to dryness, adding 5ml of water into residues to dissolve, cooling, passing through a D101 type macroporous adsorption resin column (the inner diameter is 1.5cm, the column height is 12cm), eluting with 50ml of water, discarding the water solution, eluting with 30ml of 40% ethanol, discarding the eluent, further eluting with 80ml of 70% ethanol, collecting the eluent, evaporating to dryness, dissolving the residues with methanol, transferring to a 5ml measuring flask, adding methanol to the scale, and shaking uniformly to.
The determination method comprises precisely sucking 10 μ l and 20 μ l of reference solution and 20 μ l of test solution, respectively, injecting into liquid chromatograph, determining, and calculating with logarithmic equation by external standard two-point method.
The results show that: the average content of astragaloside in the radix astragali wall-broken decoction pieces is 0.15% and not less than 0.040%.
(2) Calycosin glucoside
Octadecylsilane chemically bonded silica is used as a filler in chromatographic conditions and system applicability tests; acetonitrile is used as a mobile phase A; taking 0.2% formic acid solution as mobile phase B; gradient elution was performed as specified in the table below; the detection wavelength was 260 nm. The number of theoretical plates is not less than 3000 calculated according to calycosin glucoside peak.
Preparation of reference substance solution A proper amount of calycosin glucoside reference substance is precisely weighed, and methanol is added to prepare a solution containing 50 μ g of calycosin glucoside per 1 ml.
Preparing a test solution, precisely weighing about 1g of the product, placing the product in a round-bottom flask, precisely adding 50ml of methanol, weighing, heating and refluxing for 4 hours, cooling, weighing again, complementing the weight loss with methanol, shaking up, filtering, precisely weighing 25ml of subsequent filtrate, recovering the solvent till the residue is dry, dissolving the residue with methanol, transferring to a 5ml measuring flask, adding methanol to the scale, and shaking up to obtain the test solution.
The determination method comprises precisely sucking 10 μ l of each of the reference solution and the sample solution, injecting into liquid chromatograph, and determining. The results are shown in Table 16:
TABLE 16 determination result of cell wall-broken radix astragali decoction pieces
The results show that: the average content of calycosin glucoside in the radix astragali wall-broken decoction pieces is 0.0325%, not less than 0.020%.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The specification and examples are exemplary only.
Claims (10)
1. A quality detection method of wall-broken decoction pieces is characterized by comprising the following steps:
(1) an identification step, which comprises character identification and chromatographic identification; and
(2) the inspection step comprises the following steps of measuring the following indexes of the wall-broken decoction pieces: moisture, ash, particle size distribution, limit of unbroken cells, residual sulfur dioxide, and limit of microorganisms.
2. The quality detection method according to claim 1, wherein the property identification in the identification step comprises taking the tested wall-broken decoction pieces to be 1-10 cm2Spreading on smooth paper, flattening the surface, observing in bright place, and identifying whether the color is uniform and whether pattern color spot exists;
the chromatographic identification in the identification step comprises respectively spotting the wall-broken decoction pieces to be tested, the reference medicinal materials and the reference substance on the same thin-layer plate, placing in a developing container pre-saturated with developing agent, developing, and determining whether spots with the same color are present in the chromatogram of the wall-broken decoction pieces to be tested and the corresponding positions of the chromatogram of the reference medicinal materials and the chromatogram of the reference substance by ultraviolet lamp or sunlight inspection, wherein the thin-layer plate is selected from silica gel G thin-layer plate, silica gel GF thin-layer plate254Thin layer plate, silica gel H thin layer plate, silica gel HF254At least one of a laminate sheet and a polyamide laminate sheet.
3. The quality inspection method according to claim 1, wherein in the step (2), the moisture is measured by the following method:
taking 2-5 g of wall-broken decoction pieces as a test sample, flatly paving the test sample in a flat weighing bottle which is dried to constant weight, wherein the thickness is not more than 5mm, the loose test sample is not more than 10mm, precisely weighing, opening a bottle cap, drying for 5 hours at 100-105 ℃, covering the bottle cap, moving the bottle cap into a dryer, cooling for 30 minutes, precisely weighing, drying for 1 hour at the temperature, cooling, weighing until the difference between two successive weighing is not more than 5mg, and calculating the water content in percent in the test sample according to the weight loss.
4. The method of claim 1, wherein in step (2), the ash content is measured by a method comprising:
taking the wall-broken decoction pieces as a test sample, placing the test sample in a crucible which is burned to constant weight, weighing the test sample, slowly heating the test sample to 500-600 ℃ until the test sample is completely carbonized, gradually raising the temperature to 500-600 ℃ so as to completely ash the test sample to constant weight to obtain ash, and calculating the ash content in percent in the test sample according to the weight of residues; optionally, further comprising: and (2) adding 10ml of dilute hydrochloric acid into the ash in a crucible by a small center, covering the crucible with a surface dish, heating the crucible on a water bath for 10 minutes, flushing the surface dish with 5ml of hot water, merging washing liquor into the crucible, filtering the washing liquor by ashless filter paper, washing residues in the crucible on the filter paper by water until the washing liquor does not show chloride reaction, moving the filter residues and the filter paper into the same crucible, drying and burning the filter residues to constant weight, and calculating the content of acid-insoluble ash in percentage in the test sample according to the weight of the residues.
5. The method of claim 1, wherein the particle size distribution is determined by the following method: taking the wall-broken decoction pieces, measuring the particle size of the powder with a laser particle size analyzer, and taking the D90 value as the index of particle size distribution, wherein the particle size distribution D90 should not be more than 45 μm.
6. The quality inspection method according to claim 1, wherein the limit of unbroken cells is determined by the following method:
taking 0.01g of wall-broken decoction pieces, adding 0.5ml of chloral hydrate test solution and water in a ratio of 1:1, performing ultrasonic treatment until the wall-broken decoction pieces are completely dissolved, sucking all the solution and loading the solution into tablets, wherein the granules are not overflowed, have no bubbles and are uniformly distributed, and the number of the complete cells with the diameter of more than 100 mu m is not more than 100 when the tablets are inspected by a 100-fold microscope.
7. The quality inspection method according to claim 1, wherein the residual amount of sulfur dioxide is measured by the following method:
taking 10g of wall-broken decoction pieces, precisely weighing, placing the wall-broken decoction pieces in a two-neck round-bottom flask, adding 300-400 ml of water, opening a reflux condenser tube to supply water, connecting a rubber air duct at an E port at the upper end of the condenser tube to the bottom of a 100ml conical flask, adding 50ml of 3% hydrogen peroxide solution into the conical flask to serve as absorption liquid, adding 3 drops of 2.5mg/ml methyl red ethanol solution indicator into the absorption liquid before use, titrating the solution to yellow by using 0.01mol/L sodium hydroxide titration solution, introducing nitrogen, and adjusting the gas flow to 0.2L/min by using a flow meter; opening a piston of the separating funnel C, enabling 6mol/L hydrochloric acid solution to flow into a distillation flask, immediately heating the solution in the two-neck flask to boil, and keeping slight boiling; after the water in the flask is boiled for 1.5 hours, the heating is stopped, the absorption liquid is placed on a magnetic stirrer for continuous stirring after being cooled down, the titration is carried out by using 0.01mol/L sodium hydroxide titration solution until the yellow duration time is 20 seconds and the titration result is corrected by using a blank experiment.
8. The quality detection method according to claim 1, wherein the index of the wall-broken decoction pieces measured in the step of examining further comprises heavy metal and harmful element or pesticide residue, and the method for measuring heavy metal and harmful element is selected from heavy metal examination method or lead, cadmium, arsenic, mercury, copper assay method; or
The method for measuring the pesticide residue is selected from the group consisting of an organic chlorine pesticide residue measuring method-chromatography, an organic phosphorus pesticide residue measuring method-chromatography, a pyrethroid pesticide residue measuring method-chromatography and a pesticide residue measuring method-mass spectrometry.
9. The method of claim 1, wherein the microbial limit is determined by a method selected from the group consisting of a microbial count method and a controlled bacteria assay method.
10. The quality inspection method according to claim 1, further comprising (3) extract measurement and/or (4) active ingredient content measurement; wherein:
the extract determination comprises water-soluble extract determination, alcohol-soluble extract determination and volatile ether extract determination;
the content determination of the active ingredients comprises the following steps:
a. high performance liquid chromatography: octadecylsilane chemically bonded silica is used as a filling agent; methanol-water, acetonitrile-phosphoric acid and acetonitrile-formic acid are taken as mobile phases; at a particular detection wavelength; preparing a reference substance solution and a test solution from the reference substance and the test solution, respectively and precisely sucking the reference substance solution and the test solution, injecting the reference substance solution and the test solution into a liquid chromatograph, eluting by using a mobile phase, and measuring; or
b. Uv-vis spectrophotometry: preparing a reference substance solution and a test solution from the reference substance and the test substance; preparation of a standard curve: respectively and precisely measuring reference substance solutions with different proportions, placing the reference substance solutions in a test tube with a plug, preparing, taking a corresponding reagent as a blank, placing the prepared solution in a quartz absorption cell, measuring absorbance within the wavelength range of 190-800 nm, drawing a standard curve by taking the absorbance as a vertical coordinate and the concentration as a horizontal coordinate, precisely measuring a corresponding sample solution, performing the same operation according to the preparation method of the standard curve, measuring the absorbance, reading the content of a substance to be measured in the sample solution from the standard curve, and calculating to obtain the test substance.
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Application publication date: 20201218 |
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