CN102998273A - Quality controlling method for termitarium capsules - Google Patents
Quality controlling method for termitarium capsules Download PDFInfo
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- CN102998273A CN102998273A CN2012103042844A CN201210304284A CN102998273A CN 102998273 A CN102998273 A CN 102998273A CN 2012103042844 A CN2012103042844 A CN 2012103042844A CN 201210304284 A CN201210304284 A CN 201210304284A CN 102998273 A CN102998273 A CN 102998273A
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Abstract
The invention provides a quality controlling method for termitarium capsules. The quality controlling method comprises trait, ultraviolet identification, thin-layer identification and content measurement. The content measurement is implemented as follows: the content of total amino acids at the 570nm wavelength of an ultraviolet spectrophotometer by using amino acids as a contrast. The quality controlling method for the termitarium capsules is high in precision, good in reproducibility, low in detection cost and strong in operability, and can be used for effectively ensuring the quality of the termitarium capsules.
Description
Technical field
The invention belongs to the Chinese medicine preparation field of quality control, particularly a kind of method of quality control of termitarium capsule.
Background technology
Termitarium is the dry body of termite colony and fungus garden thereof.Wherein, termite mainly is Odontotermes formosanus (Odontotermes formosanus Shiraki) or yellow-wing subterranean termite (Macrotermes barneyi Light), and fungus garden is take collybia albuminosa (Termitomyces albuminosus (Berk) Heim) as main.The medical value of relevant termite and fungus garden thereof, existing correlative study and report in traditional Chinese medicine.Li Shizhen (1518-1593 A.D.) is write in Compendium of Material Medica: " termite mud, purport is disliked pyogenic infections from tumour or sore, and with person on the pine, each is fried and deceives with yellow lead, grinds with fragrant stain and is coated with it, getting more is to end ", " smell is sweet, flat, nontoxic for collybia albuminosa.Cure mainly beneficial stomach, clear refreshing, control hemorrhoid "." middle traditional Chinese medicines sea " points out that also its meridian distribution of property and flavor is " sweet, flat.Nontoxic.Enter the heart, lung, spleen three warps, it is refreshing clearly to cure mainly strengthening the spleen and stomach, beneficial gas.”
The several amino acids and the various trace elements that contain needed by human body in the termitarium wherein mainly contain following amino acid: ornithine, aspartic acid, threonine, serine, glutamic acid, proline, glycocoll, alanine, cystine, valine, methionine, isoleucine, leucine, tyrosine, phenylalanine, lysine, histidine, arginine and aminobutyric acid etc.But proline accelerating wound.It is the adrenergic raw material of preparation thyroxine that tyrosine can be treated hepatic coma.L-asparagus fern amino-acid salt is used for the treatment of liver illness and protection cardiac muscle and antifatigue etc.Leucine lacks can make complement C3 level descend, and isoleucine lacks the transferrin level that only makes in the animal peritoneal exudate and descends.Arginine is still treated the common medicine of the male sterility of sperm deficiency.Aminobutyric acid has many-sided physiologically active, except hypotensive, anticonvulsion, diuresis, hemangiectasis, as amino acid whose transmission matter and promote the brain metabolism.
CN951077287 discloses a kind of pharmaceutical composition and application thereof that comprises termite population and main nest bacterial nursery thereof, and this pharmaceutical composition has the effect of the various diseases such as treatment chronic hepatitis, anti-inflammatory analgesic, treatment of arthritis, infertility.CN102138940 discloses a kind of production method of termitarium capsule, the termitarium capsule good effect that the method prepares, has no side effect, and it is many to contain effective composition, and clinical drug effect is remarkable.
Yet the quality control of existing termitarium capsule adopts qualitatively method to determine that there are the defectives such as characteristic is strong, qualitative results is inaccurate, repeatability is bad in these methods, cause the difficult quality control of existing termitarium capsule usually.
Summary of the invention
Goal of the invention: the method that the purpose of this invention is to provide the accurately termitarium capsule quality control of a kind of measurement result.
Technical scheme: the method for quality control of a kind of termitarium capsule provided by the invention, this method of quality control comprise that proterties, ultraviolet are differentiated, thin layer is differentiated, assay.
Wherein, described assay is measured the content of total amino acid for take amino acid as contrast at ultraviolet spectrophotometer 570nm wavelength place.
The method of quality control of this termitarium capsule is specially:
(1) proterties:
Described termitarium capsule 's content is brown powder; Gas is little, little acid of distinguishing the flavor of;
(2) differentiate:
Get the termitarium capsule 's content, with water-soluble solution, the amount ratio of described termitarium capsule 's content and water is 1g:10ml, dissolving in the warm 10-15 of water-bath minute, and cooling, filtration get filtrate;
Get filtrate and put on filter paper, spray is placed 2-4min with 0.25% triketohydrindene hydrate ethanol in 100 ± 10 ℃ baking oven, be the aubergine spot;
Get filtrate and put on filter paper, spray is placed 2-4min with istain reagent in 100 ± 10 ℃ baking oven, be pink spot;
Get filtrate 1ml, add 4% sodium carbonate liquor 1ml, heat 2-4min in boiling water bath, put in the ice bath and cool off, add 2 of diazotising reagent, solution takes on a red color;
(3) thin layer is differentiated:
The thin layer test sample is prepared: get the termitarium capsule 's content, with the ultrasonic extraction of water 15-30min, described termitarium capsule 's content: the amount ratio of water is 1g:10ml, filters, and namely gets the thin layer need testing solution;
Take leucine aqueous solution, glutamic acid aqueous solution as contrast, thin layer need testing solution and contrast are put on silica gel thin-layer plate respectively, normal butyl alcohol: glacial acetic acid: water is developping agent, described normal butyl alcohol: glacial acetic acid: the amount ratio of water is 4: 1: 1, spray develops the color with 0.25% triketohydrindene hydrate ethanol, in 100 ± 10 ℃ baking oven, place 2-4min, be the aubergine spot;
(4) total amino acid assay:
Reference substance solution is prepared: get amino acid reference substance 0.2g, and accurately weighed, put in the 100ml measuring bottle, be dissolved in water, constant volume, precision is measured 10ml, places the 100ml measuring bottle, and constant volume namely gets reference substance solution; The concentration of this reference substance solution is 200 μ g/ml;
The preparation of typical curve: precision is measured reference substance solution 0.0ml, 0.5ml, 1.0ml, 1.5ml, 2.0ml, 2.5ml, 3.0mL, place respectively the 25ml measuring bottle, add water to 4ml, the ninhydrin solution of adding 20g/L and pH are each 1mL of phosphate buffered solution of 8.04, mixing, heating water bath 15min, take out and be chilled to rapidly room temperature, add water to scale, shake up, leave standstill 15min, under the 570nm wavelength, take the 0ml reference substance solution as blank, with ultraviolet spectrophotometry, measure absorbance at 570nm wavelength place, take absorbance as ordinate, concentration is horizontal ordinate drawing standard curve;
Assay method: get the termitarium capsule 's content, with water-soluble solution, the amount ratio of described termitarium capsule 's content and water is 2g:100ml, and is accurately weighed, ultrasonic 10-15min, and cooling is supplied weight with water; The accurate 2ml that draws places the 25ml measuring bottle, adds water to 4ml, and the ninhydrin solution of adding 20g/L and pH are each 1mL of phosphate buffered solution of 8.04, mixing, and heating water bath 15min takes out and is chilled to rapidly room temperature, adds water to scale, shakes up, and leaves standstill 15min; Take the 0ml reference substance solution as blank, with ultraviolet spectrophotometry, measure absorbance at 570nm wavelength place, according to typical curve, calculate total amino acid content.
Beneficial effect: the method for quality control precision height of termitarium capsule provided by the invention, favorable reproducibility, testing cost are low, workable, can effectively guarantee the quality of termitarium capsule.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is made and to further specify.
Embodiment 1 termitarium capsule total amino acid content assaying method is investigated.
(1) instrument and reagent:
TU-1901 type ultraviolet spectrophotometer Beijing all purpose instrument equipment company limited
Examine institute in the leucine reference substance
Three batches of termitarium capsule samples, self-control; Batch 1, batches 2 and batches 3.
(2) solution is prepared:
Reference substance solution is prepared: get leucine reference substance 0.2005g, and accurately weighed, put in the 100ml measuring bottle, be dissolved in water, constant volume, precision is measured 10ml, places the 100ml measuring bottle, and constant volume namely gets reference substance solution; The concentration of this reference substance solution is 0.2005mg/ml.
Need testing solution is prepared: get three batches of termitarium capsule 's contents, with water-soluble solution, the amount ratio of described termitarium capsule 's content and water is 2g:100ml, and is accurately weighed, ultrasonic 10-15min, and cooling is supplied weight with water; Namely get three batches of need testing solutions, be respectively batch 1 solution, batch 2 solution and batch 3 solution.
(3) wavelength is selected:
Get respectively reference substance solution and batch 1 solution, not add reference substance or need testing solution as negative control; The accurate 2ml that draws places the 25ml measuring bottle, adds water to 4ml, and the ninhydrin solution of adding 20g/L and pH are each 1mL of phosphate buffered solution of 8.04, mixing, and heating water bath 15min takes out and is chilled to rapidly room temperature, adds water to scale, shakes up, and leaves standstill 15min; In the interscan of 250-600 wavelength coverage, reference substance solution and need testing solution have absorption maximum at wavelength 570nm place, and negative control at this wavelength without obvious absorption, therefore select 570nm to detect wavelength.
(4) preparation of typical curve:
Precision is measured reference substance solution 0.0ml, 0.5ml, 1.0ml, 1.5ml, 2.0ml, 2.5ml, 3.0mL, place respectively the 25ml measuring bottle, add water to 4ml, the ninhydrin solution of adding 20g/L and pH are each 1mL of phosphate buffered solution of 8.04, mixing, heating water bath 15min, take out and be chilled to rapidly room temperature, add water to scale, shake up, leave standstill 15min; Take the 0ml reference substance solution as blank, with ultraviolet spectrophotometry, measure absorbance at 570nm wavelength place, take absorbance as ordinate, concentration is horizontal ordinate drawing standard curve; The gained typical curve is A=0.0256C-0.0003(R
2=0.9999) wherein A is absorbance, and C is leucine concentration.Measurement result sees Table 1.
Table 1 leucine reference substance typical curve is investigated
| Sequence number | Reference substance solution amount ml | Concentration μ g/ml | Absorbance |
| 1 | 0.5 | 4.01 | 0.102 |
| 2 | 1.0 | 8.02 | 0.202 |
| 3 | 1.5 | 12.03 | 0.309 |
| 4 | 2.0 | 16.04 | 0.413 |
| 5 | 2.5 | 20.05 | 0.511 |
| 6 | 3.0 | 24.06 | 0.613 |
(5) Precision Experiment
Get reference substance solution No. 3, with standard curve determination method replication 5 times, the record absorbance, and calculate standard deviation, the result shows that it is good that the reference substance leucine is measured precision.See Table 2.
Table 2 Precision test result
(6) stability test
Get batch 1 a solution 2ml, at set intervals with standard curve determination method replication, record absorbance under the room temperature, and calculate standard deviation, the result shows that the sample total amino acid is measured good stability.See Table 3.
Table 3 stability test result
(7) replica test
Get batch 1 a solution 2ml, with standard curve determination method replication 5 times, the record absorbance, and calculate standard deviation, the result shows that the sample total amino acid is measured good reproducibility.See Table 4.
Table 4 replica test result
The control of embodiment 2 termitarium capsule qualities.
(1) termitarium capsule proterties:
Described termitarium capsule 's content is brown powder; Gas is little, little acid of distinguishing the flavor of;
(2) differentiate:
Get the termitarium capsule 's content, with water-soluble solution, the amount ratio of described termitarium capsule 's content and water is 1g:10ml, dissolving in the warm 10-15 of water-bath minute, and cooling, filtration get filtrate;
Get filtrate and put on filter paper, spray is placed 2-4min with 0.25% triketohydrindene hydrate ethanol in 100 ± 10 ℃ baking oven, be the aubergine spot;
Get filtrate and put on filter paper, spray is placed 2-4min with istain reagent in 100 ± 10 ℃ baking oven, be pink spot;
Get filtrate 1ml, add 4% sodium carbonate liquor 1ml, heat 2-4min in boiling water bath, put in the ice bath and cool off, add 2 of diazotising reagent, solution takes on a red color;
This shows that the termitarium capsule contains principal ingredient amino acid.
(3) thin layer is differentiated:
The thin layer test sample is prepared: get the termitarium capsule 's content, with the ultrasonic extraction of water 15-30min, described termitarium capsule 's content: the amount ratio of water is 1g:10ml, filters, and namely gets the thin layer need testing solution;
Take leucine aqueous solution, glutamic acid aqueous solution as contrast, thin layer need testing solution and contrast are put on silica gel thin-layer plate respectively, normal butyl alcohol: glacial acetic acid: water is developping agent, described normal butyl alcohol: glacial acetic acid: the amount ratio of water is 4: 1: 1, spray develops the color with 0.25% triketohydrindene hydrate ethanol, in 100 ± 10 ℃ baking oven, place 2-4min, be the aubergine spot;
The result shows, the termitarium capsule contain leucine, glutamic acid and with leucine and glutamic acid colour developing point position near the close point of color, can judge that thus the termitarium capsule contains several amino acids.
(4) total amino acid assay:
Get sample to be tested 2ml, place the 25ml measuring bottle, add water to 4ml, the ninhydrin solution of adding 20g/L and pH are each 1mL of phosphate buffered solution of 8.04, mixing, and heating water bath 15min takes out and is chilled to rapidly room temperature, adds water to scale, shakes up, and leaves standstill 15min; Take the 0ml reference substance solution as blank, with ultraviolet spectrophotometry, measure absorbance at 570nm wavelength place, calculate total amino acid content.
Batch 1 solution, batch 2 solution and batch 3 solution are respectively measured respectively three times, the results are shown in Table 5.
Table 5 total amino acid assay result
Claims (3)
1. the method for quality control of a termitarium capsule is characterized in that: this method of quality control comprises that proterties, ultraviolet are differentiated, thin layer is differentiated, assay.
2. the method for quality control of a kind of termitarium capsule according to claim 1 is characterized in that: described assay is measured the content of total amino acid for take amino acid as contrast at ultraviolet spectrophotometer 570nm wavelength place.
3. the method for quality control of a kind of termitarium capsule according to claim 1 is characterized in that: may further comprise the steps:
(1) proterties:
Described termitarium capsule 's content is brown powder; Gas is little, little acid of distinguishing the flavor of;
(2) differentiate:
Get the termitarium capsule 's content, with water-soluble solution, the amount ratio of described termitarium capsule 's content and water is 1g:10ml, dissolving in the warm 10-15 of water-bath minute, and cooling, filtration get filtrate;
Get filtrate and put on filter paper, spray is placed 2-4min with 0.25% triketohydrindene hydrate ethanol in 100 ± 10 ℃ baking oven, be the aubergine spot;
Get filtrate and put on filter paper, spray is placed 2-4min with istain reagent in 100 ± 10 ℃ baking oven, be pink spot;
Get filtrate 1ml, add 4% sodium carbonate liquor 1ml, heat 2-4min in boiling water bath, put in the ice bath and cool off, add 2 of diazotising reagent, solution takes on a red color;
(3) thin layer is differentiated:
The thin layer test sample is prepared: get the termitarium capsule 's content, with the ultrasonic extraction of water 15-30min, described termitarium capsule 's content: the amount ratio of water is 1g:10ml, filters, and namely gets the thin layer need testing solution;
Take leucine aqueous solution, glutamic acid aqueous solution as contrast, thin layer need testing solution and contrast are put on silica gel thin-layer plate respectively, normal butyl alcohol: glacial acetic acid: water is developping agent, described normal butyl alcohol: glacial acetic acid: the amount ratio of water is 4: 1: 1, spray develops the color with 0.25% triketohydrindene hydrate ethanol, in 100 ± 10 ℃ baking oven, place 2-4min, be the aubergine spot;
(4) total amino acid assay:
Reference substance solution is prepared: get amino acid reference substance 0.2g, and accurately weighed, put in the 100ml measuring bottle, be dissolved in water, constant volume, precision is measured 10ml, places the 100ml measuring bottle, and constant volume namely gets reference substance solution; The concentration of this reference substance solution is 200 μ g/ml;
The preparation of typical curve: precision is measured reference substance solution 0.0ml, 0.5ml, 1.0ml, 1.5ml, 2.0ml, 2.5ml, 3.0mL, place respectively the 25ml measuring bottle, add water to 4ml, the ninhydrin solution of adding 20g/L and pH are each 1mL of phosphate buffered solution of 8.04, mixing, heating water bath 15min, take out and be chilled to rapidly room temperature, add water to scale, shake up, leave standstill 15min, under the 570nm wavelength, take the 0ml reference substance solution as blank, with ultraviolet spectrophotometry, measure absorbance at 570nm wavelength place, take absorbance as ordinate, concentration is horizontal ordinate drawing standard curve;
Assay method: get the termitarium capsule 's content, with water-soluble solution, the amount ratio of described termitarium capsule 's content and water is 2g:100ml, and is accurately weighed, ultrasonic 10-15min, and cooling is supplied weight with water; The accurate 2ml that draws places the 25ml measuring bottle,, add water to 4ml, the ninhydrin solution of adding 20g/L and pH are each 1mL of phosphate buffered solution of 8.04, mixing, heating water bath 15min takes out and is chilled to rapidly room temperature, adds water to scale, shakes up, and leaves standstill 15min; Take the 0ml reference substance solution as blank, with ultraviolet spectrophotometry, measure absorbance at 570nm wavelength place, according to typical curve, calculate total amino acid content.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108061766A (en) * | 2017-12-05 | 2018-05-22 | 江西中医药大学 | A kind of method of quality control of Fructus Hordei Germinatus granule |
| CN109283025A (en) * | 2018-09-18 | 2019-01-29 | 苏州太湖美药业有限公司 | The detection method of contained polypeptide classes in a kind of pearl powder |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1818642A (en) * | 2006-03-23 | 2006-08-16 | 江西汇仁药业有限公司 | Quality Controlling method of Qianlieshule preparation |
| CN1857445A (en) * | 2006-03-23 | 2006-11-08 | 江西汇仁药业有限公司 | Quality control method for Desheng preparation |
| CN1931343A (en) * | 2006-09-12 | 2007-03-21 | 佘广宇 | Quality standard and inspection method for coronary heart disease treating medicine tablet of seven ingredients |
-
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- 2012-08-23 CN CN201210304284.4A patent/CN102998273B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1818642A (en) * | 2006-03-23 | 2006-08-16 | 江西汇仁药业有限公司 | Quality Controlling method of Qianlieshule preparation |
| CN1857445A (en) * | 2006-03-23 | 2006-11-08 | 江西汇仁药业有限公司 | Quality control method for Desheng preparation |
| CN1931343A (en) * | 2006-09-12 | 2007-03-21 | 佘广宇 | Quality standard and inspection method for coronary heart disease treating medicine tablet of seven ingredients |
Non-Patent Citations (1)
| Title |
|---|
| 汤明辉等: "复方玉驹胶囊的质量标准研究", 《华西药学杂志》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108061766A (en) * | 2017-12-05 | 2018-05-22 | 江西中医药大学 | A kind of method of quality control of Fructus Hordei Germinatus granule |
| CN109283025A (en) * | 2018-09-18 | 2019-01-29 | 苏州太湖美药业有限公司 | The detection method of contained polypeptide classes in a kind of pearl powder |
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