CN110780018A - Quality control method of Jinggan granules - Google Patents
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Abstract
The invention relates to the field of quality standards of traditional Chinese medicine preparations, in particular to a quality control method of liver-cleaning granules, which comprises the following steps: 1) identifying giant knotweed; 2) identifying the salvia miltiorrhiza; 3) detecting the content of emodin and chrysophanol. The quality control method can effectively control the active ingredients of the liver-essence granules, has the characteristics of stability, reliability, strong specificity, high precision, good reproducibility, high recovery rate and accurate measurement result, achieves the aim of ensuring the quality of the liver-essence granules, ensures the exertion of the curative effect and has good clinical application prospect.
Description
Technical Field
The invention relates to the field of quality standards of traditional Chinese medicine preparations, in particular to a quality control method of liver-nourishing granules.
Background
The liver and kidney granules are a traditional Chinese medicine preparation for the adjuvant therapy of hepatitis symptoms, have the efficacies of clearing heat and promoting diuresis, cooling blood and detoxifying, and are suitable for the adjuvant therapy of symptoms such as yellow body and eyes, bright color, yellow urine, fullness in chest and epigastrium or hypochondrium pain, anorexia, dry mouth and bitter taste, constipation and the like caused by liver and gallbladder damp-heat.
However, the quality standard of the liver-essence granules is not perfect at present, the control method is poor in stability, the specificity is high, the limitation is large, the quality of the liver-essence granules is difficult to accurately control, and the liver-essence granules are limited in the aspects of the therapeutic effect and the clinical application prospect.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide the quality control method of the liver-clearing granules, which can effectively control the active ingredients of the liver-clearing granules, is stable and reliable, has strong specificity, can achieve the aim of ensuring the quality of the liver-clearing granules, thereby ensuring the exertion of the curative effect and having good clinical application prospect.
The purpose of the invention is realized by the following technical scheme: a quality control method of JINGGANKE granule comprises the following steps: 150g of oriental wormwood, 150g of giant knotweed rhizome, 100g of lithospermum, 100g of rhubarb, 100g of amur corktree bark, 100g of red paeony root, 100g of salvia miltiorrhiza, 100g of turmeric root-tuber and 60g of liquorice.
The quality detection method of the liver-nourishing granules comprises the following steps:
1) identification of giant knotweed rhizome: taking 4g of liver essence granules, grinding, adding 25-35ml of water, carrying out ultrasonic treatment at the frequency of 45-60Hz for 25-34min, filtering, extracting the filtrate with chloroform for 2 times, 8-12ml each time, discarding the chloroform solution, extracting with ethyl acetate for 2 times, 8-12ml each time, combining the ethyl acetate solutions obtained by the extraction for 2 times, evaporating to dryness, and adding 0.5-1.5ml of methanol for dissolving to obtain a sample solution; adding methanol into polydatin to obtain polydatin solution of 0.8-1.2mg/ml, taking as reference solution, sucking test solution and reference solution 0.8-1.2 μ l respectively by thin layer chromatography, and respectively dropping on the same silica gel GF
254Developing the liquid to be detected by using a first developing agent on the thin-layer plate until the distance is 8-15 cm, taking out, drying, placing under an ultraviolet lamp with the wavelength of 254 +/-2 nm for inspection, and displaying fluorescent spots with the same color in the chromatogram of the test sample at the position corresponding to the chromatogram of the reference substance;
2) identification of salvia miltiorrhiza: collecting refined liver granule 10g, grinding, adding 15-25ml methanol, ultrasonic treating at 45-60Hz frequency for 25-35min, filtering, evaporating filtrate, dissolving in 15-25ml water, adjusting pH to 2 with hydrochloric acid-4, extracting with ethyl acetate for 3 times, 15-25ml each time, combining ethyl acetate solutions for 3 times of extraction, evaporating to dryness, and dissolving with 0.5-1.5ml anhydrous ethanol to obtain a test solution; adding methanol into salvianolic acid B to obtain 1-2mg/ml salvianolic acid B solution as reference solution, performing thin layer chromatography, sucking 2-4 μ l sample solution and 1-3 μ l reference solution, and respectively dropping on the same silica gel GF
254Developing the liquid to be detected by using a second developing agent on the thin-layer plate until the distance is 8-15 cm, taking out, drying, and inspecting under an ultraviolet lamp with the wavelength of 254 +/-2 nm to show fluorescent spots with the same color in the chromatogram of the test sample at the position corresponding to the chromatogram of the reference sample;
3) detecting the content of emodin and chrysophanol:
(1) liquid chromatography conditions: the chromatographic conditions for determining emodin and chrysophanol are that octadecylsilane chemically bonded silica is used as filler; methanol-phosphoric acid with the concentration of 0.08-0.12% is used as a mobile phase according to the volume ratio of 90: 10; the detection wavelength is 254 +/-2 nm; the flow rate is 1.0 ml/min; column temperature: 25 ℃;
the theoretical plate number is determined according to the following steps: under the test conditions, the theoretical plate number is specified to be 2000-5000 in the system applicability test;
(2) preparation of control solutions: accurately weighing appropriate amount of emodin and chrysophanol reference substances, dissolving with methanol to obtain mixed solution containing emodin 5.46 μ g and chrysophanol 0.992 μ g per 1ml, and storing in dark place;
(3) preparing a test solution, precisely weighing 1g of fine liver particles, placing the fine liver particles in a conical flask, precisely adding 45-55ml of methanol, weighing, heating and refluxing for 25-35min, cooling, weighing again, complementing the weight loss by methanol, shaking uniformly, filtering, precisely weighing 4.8-5.2ml of subsequent filtrate, placing the subsequent filtrate in a 50ml round-bottomed flask, volatilizing ethanol, adding 10ml of 2.5mol/L sulfuric acid solution, performing ultrasonic treatment for 4-6min, adding 10ml of chloroform, heating and refluxing for 55-65min, cooling, transferring to a separating funnel, washing a container by a small amount of chloroform, merging into the separating funnel, separating a chloroform layer, extracting acid liquid by chloroform for 2 times, 9-11ml each time, merging chloroform liquid, dehydrating by anhydrous sodium sulfate, transferring the chloroform liquid to a 100ml conical flask, volatilizing chloroform, precisely adding 8-12ml of methanol, weighing, placing the subsequent liquid in a water bath for slightly heating and dissolving, cooling, complementing the weight loss by methanol, adding the filtrate to a 100ml conical flask, shaking uniformly, taking the chloroform, precisely adding 8-12ml of methanol, weighing, placing the residual liquid in a pure HPLC chromatographic instrument for obtaining pure chrysophanol, and detecting the pure liquid phase by a 11032 μm chromatographic column, wherein the pure HPLC chromatographic detector is used for detecting the pure liquid phase of a pure HPLC chromatographic instrument for detecting the pure chrysophanol, and the pure HPLC (11032), and the HPLC) for detecting the pure liquid chromatography, and the purity of the pure chrysophanol, and the HPLC chromatography is preferably used for detecting the detection of a 11032 μm chromatographic instrument for detecting the detection sample by a 11032. medium, and the detection sample is used as a detection instrument for detecting the detection sample with a detection instrument for detecting;
(4) the determination method comprises the following steps: precisely sucking 10 μ l of each of the reference solution and the sample solution, injecting into liquid chromatograph, and measuring.
Preferably, in the step 1), the first developing agent used in the development is a mixture of chloroform-acetone-formic acid-water according to a volume ratio of 3-5:4:0.4-0.6: 0.1-0.3.
Preferably, in the step 2), the second developing agent used in the development is a mixture of toluene-ethyl acetate-formic acid according to a volume ratio of 1.8-2.2:5.8-6.2: 0.8-1.2.
The invention has the beneficial effects that: the quality control method can effectively control the active ingredients of the liver-essence granules, has the characteristics of stability, reliability, strong specificity, high precision, good reproducibility, high recovery rate and accurate measurement result, achieves the aim of ensuring the quality of the liver-essence granules, ensures the exertion of the curative effect and has good clinical application prospect.
Drawings
FIG. 1 is a thin-layer chromatogram for identification of liver essence granule rhizoma Polygoni Cuspidati; wherein, 1 is lacking rhizoma Polygoni Cuspidati JINGGAN granule, 2 is JINGGAN granule, 3 is rhizoma Polygoni Cuspidati control, 4 is JINGGAN granule, and 5 is JINGGAN granule;
FIG. 2 is a thin-layer chromatogram of radix Salviae Miltiorrhizae for identifying liver and kidney essence granule; wherein, 1 is lack of radix salviae miltiorrhizae and liver-essence granule, 2 is liver-essence granule, 3 is radix salviae miltiorrhizae reference substance, 4 is liver-essence granule, and 5 is liver-essence granule;
FIG. 3 is an HPLC chromatogram of an emodin control;
FIG. 4 is an HPLC chromatogram of chrysophanol control;
FIG. 5 is a HPLC chromatogram of a test sample;
FIG. 6 is a negative sample HPLC profile;
FIG. 7 is an emodin standard curve;
fig. 8 is a chrysophanol standard curve.
Detailed Description
For the understanding of those skilled in the art, the present invention will be further described with reference to the following examples and accompanying drawings 1 to 8, and the content of the embodiments is not intended to limit the present invention.
Examples
The formula of the liver-nourishing granules comprises: 150g of oriental wormwood, 150g of giant knotweed rhizome, 100g of lithospermum, 100g of rhubarb, 100g of amur corktree bark, 100g of red paeony root, 100g of salvia miltiorrhiza, 100g of turmeric root-tuber and 60g of liquorice.
A quality control method of liver-essence granules comprises the following steps:
1) identification of giant knotweed rhizome: taking 4g of liver essence granules, grinding, adding 30ml of water, carrying out ultrasonic treatment for 30min at the frequency of 50Hz, filtering, extracting the filtrate for 2 times by using trichloromethane, 10ml each time, discarding the trichloromethane solution, extracting for 2 times by using ethyl acetate, 10ml each time, combining the ethyl acetate solutions used for 2 times of extraction, evaporating to dryness, and adding 1.0ml of methanol for dissolving to obtain a sample solution; adding methanol into polydatin to obtain 1.0mg/ml polydatin solution as reference solution, and dropping the solution into the same silica gel GF by thin layer chromatography
254Developing the solution to be detected by using a mixed developing agent consisting of trichloromethane-acetone-formic acid-water according to the volume ratio of 4:4:0.5:0.2 on a thin layer plate, taking out when the solution to be detected is developed to a distance of 10cm, airing, and placing under an ultraviolet lamp with the wavelength of 254nm for inspection, wherein fluorescent spots with the same color appear on the positions, corresponding to the color spectrum of a reference substance, of the color spectrum of the sample;
2) identification of salvia miltiorrhiza: collecting refined liver granule 10g, grinding, adding 20ml methanol, ultrasonic treating at 50Hz frequency for 30min, filtering, evaporating filtrate, dissolving in 20ml water, adjusting pH to 3 with hydrochloric acid, and adding ethyl acetateExtracting for 3 times (20 ml each time), mixing ethyl acetate solutions obtained by extracting for 3 times, evaporating to dryness, and dissolving with 1.0ml anhydrous ethanol to obtain sample solution; adding methanol into salvianolic acid B to obtain 1.5mg/ml salvianolic acid B solution as reference solution, performing thin layer chromatography, sucking 4 μ l of sample solution and 2 μ l of reference solution, and respectively dropping on the same silica gel GF
254Developing the solution to be detected by using a mixed developing agent consisting of toluene, ethyl acetate and formic acid according to the volume ratio of 2:6:1.0 on a thin-layer plate, taking out the solution to be detected when the solution is developed to a distance of 10cm, airing the solution, and placing the solution under an ultraviolet lamp with the wavelength of 254nm for inspection, wherein fluorescent spots with the same color appear in the chromatogram of the test solution at positions corresponding to the chromatogram of the reference solution;
3) detecting the content of emodin and chrysophanol:
(1) instruments and reagents: the high performance liquid chromatograph is Waters515 HPLC; the chromatographic column is a Hypersil C18(5 μm, 250X 4.6mm) Waters2487 dual-wavelength ultraviolet detector; the methanol is chromatographic pure, the water is ultrapure water, and other reagents are analytical pure;
(2) purity and source of the reference: emodin and chrysophanol are provided by the verification of Chinese medicine biological products and are used for content determination, and the batch numbers are respectively as follows: 110756, 201110, 110796, 201310;
(3) liquid chromatography conditions: the chromatographic conditions for determining emodin and chrysophanol are that octadecylsilane chemically bonded silica is used as filler; methanol-phosphoric acid with the concentration of 0.08-0.12% is used as a mobile phase according to the volume ratio of 90: 10; the detection wavelength is 254 nm; the flow rate is 1.0 ml/min; column temperature: 25 ℃; the theoretical plate number is determined according to the following steps: under the above test conditions, the theoretical plate number was defined to be 2000 in the system suitability test;
(4) preparation of control solutions: accurately weighing appropriate amount of emodin and chrysophanol reference substances, dissolving with methanol to obtain mixed solution containing emodin 5.46 μ g and chrysophanol 0.992 μ g per 1ml, and storing in dark place;
(5) preparation of a test solution: weighing 1g of liver essence granules, precisely weighing, placing in an erlenmeyer flask, precisely adding 50ml of methanol, weighing, heating and refluxing for 30min, cooling, weighing again, complementing the lost weight with methanol, shaking, filtering, precisely weighing 5ml of subsequent filtrate, placing in a 50ml round-bottom flask, volatilizing ethanol, adding 10ml of 2.5mol/L sulfuric acid solution, ultrasonically treating for 5min, adding 10ml of chloroform, heating and refluxing for 55-65min, cooling, transferring to a separating funnel, washing the container with a small amount of chloroform, merging into the separating funnel, collecting the chloroform layer, extracting the acid solution with chloroform for 2 times, 10ml each time, combining the chloroform solution, dehydrating with anhydrous sodium sulfate, transferring the chloroform solution to a 100ml erlenmeyer flask, volatilizing chloroform, precisely adding 10ml of methanol to the residue, weighing, slightly heating and dissolving the residue in a water bath, cooling, further weighing, complementing the lost weight with methanol, shaking, filtering the supernatant with 0.45 μm microporous membrane, and collecting the filtrate;
(6) the determination method comprises the following steps: precisely sucking 10 μ l of each of the reference solution and the sample solution, injecting into a liquid chromatograph, and measuring;
(7) comparison of test solution extraction methods: weighing about 2g of the fine powder of the product, precisely weighing, placing in an erlenmeyer flask, precisely adding 50ml of methanol, weighing, respectively ultrasonically shaking and heating reflux extracting for 30 minutes, cooling, weighing again, complementing the weight loss by methanol, shaking uniformly, precisely weighing 5ml of subsequent filtrate, placing in a 50ml round-bottomed flask, volatilizing ethanol, adding 10ml of 2.5mol/L sulfuric acid solution, ultrasonically treating for 5 minutes, adding 10ml of chloroform, heating reflux for 1 hour, cooling, transferring to a separating funnel, washing the container by a small amount of chloroform, merging into the separating funnel, separately taking a chloroform layer, extracting acid liquor by chloroform for 2 times, about 10ml each time, combining chloroform solutions, dehydrating by anhydrous sodium sulfate, transferring the chloroform solution to a 100ml erlenmeyer flask, volatilizing chloroform, precisely adding 10ml of methanol to the residue, weighing, slightly heating and dissolving the residue in a water bath, cooling, complementing the weight loss by methanol, shaking, filtering the supernatant with 0.45 μm microporous membrane, collecting the filtrate, injecting sample, and comparing the extraction effects of the two extraction methods, the results are shown in Table 1;
TABLE 1 comparison of extraction methods
The peak areas of the emodin and the chrysophanol extracted by the heating reflux method are slightly larger than those extracted by the ultrasonic oscillation method, and the methanol solution extracted by the reflux method is easy to filter, so that the method of adding 25ml of methanol and heating reflux extraction for 30 minutes is adopted.
(8) Examination of the linear relationship: precisely sucking 1, 3, 5, 7 and 9 μ l of 4.5 μ g/ml control solution and 1.5 and 2.0 μ l of 0.156mg/ml control solution, respectively, injecting into a liquid chromatograph, measuring peak area, drawing a standard curve with the sample injection amount (ng) of the control as abscissa and the peak area as ordinate, and determining the results as shown in Table 2;
TABLE 2 results of Linear examination
The regression equation is that the correlation coefficient r is 0.9999 between Y and 0.0601X and 0.1125, which shows that the emodin has good linear relation in the range of the sample injection amount of 13.65ng to 109.2 ng; chrysophanol shows good linear relation in the sampling amount range of 2.48ng-19.84ng, as shown in figures 6 and 7;
(9) blank test: preparing negative particles without rhubarb and giant knotweed rhizome, preparing negative solution by the same method as the test solution, precisely sucking 10 mul of sample injection, and showing that the result is in the position range of the component to be measured, no absorption exists, thus showing that the negative solution has no interference, and being shown in figure 7.
(10) And (3) stability test: precisely sucking 10 mu l of the same test solution, and measuring the peak area of the same test solution at regular intervals, wherein the test result shows that the content of the test solution is stable within 24 hours, which is shown in Table 3;
TABLE 3 stability test knot
(11) And (3) precision test: precisely sucking 5 mul of the same reference substance solution, and repeatedly injecting the sample for 5 times, wherein the result shows that the precision of the instrument is good;
TABLE 4 results of precision test
(12) Recovery rate test: adopting sample-adding recovery method, collecting refined liver granule, respectively and precisely adding emodin and chrysophanol reference solution, measuring content according to content measurement method, and calculating recovery rate;
TABLE 5 emodin recovery determination results
TABLE 6 results of determination of chrysophanol recovery
(13) And (3) measuring the content of the test sample: preparing a test solution according to the method, and performing content measurement on ten batches of the preparation, wherein the results are shown in table 7;
TABLE 7 results of content measurement
(14) And (3) establishing a content limit standard: according to the results of the 10 batches of data, the average value of the sum of the contents of the emodin and the chrysophanol is 3.98 mg/bag, and the average content is calculated according to 80 percent, and is 3.18 mg/bag; the average content of emodin is 3.09 mg/bag, and calculated according to the average content of 80%, the content is 2.47 mg/bag; because the product content is greatly influenced by medicinal materials, batch and other factors, each bag of the tentative sperm liver granules contains giant knotweed rhizome and rhubarb, and the total content of emodin and chrysophanol is not less than 3.0 mg/bag, and the content of emodin is not less than 2.40 mg/bag.
The above-described embodiments are preferred implementations of the present invention, and the present invention may be implemented in other ways without departing from the spirit of the present invention.
Claims (7)
1. A quality control method of JINGGANKE granule comprises the following steps: 150g of oriental wormwood, 150g of giant knotweed rhizome, 100g of lithospermum, 100g of rhubarb, 100g of amur corktree bark, 100g of red paeony root, 100g of salvia miltiorrhiza, 100g of turmeric root-tuber and 60g of liquorice, and is characterized in that: the quality detection method of the liver-nourishing granules comprises the following steps:
1) identification of giant knotweed rhizome: taking 4g of liver essence granules, grinding, adding 25-35ml of water, performing ultrasonic treatment for 25-34min, filtering, extracting the filtrate with chloroform for 2 times (8-12 ml each time), discarding chloroform solution, extracting with ethyl acetate for 2 times (8-12 ml each time), mixing ethyl acetate solutions obtained by 2 times of extraction, evaporating to dryness, and dissolving with 0.5-1.5ml of methanol to obtain a sample solution; adding methanol into polydatin to obtain polydatin solution of 0.8-1.2mg/ml, taking as reference solution, sucking test solution and reference solution 0.8-1.2 μ l respectively by thin layer chromatography, and respectively dropping on the same silica gel GF
254Developing the liquid to be detected by using a first developing agent on the thin-layer plate, taking out, airing, and placing under an ultraviolet lamp for inspection, wherein fluorescent spots with the same color appear in the chromatogram of the test sample at the positions corresponding to the chromatograms of the reference sample;
2) identification of salvia miltiorrhiza: taking 10g of liver essence granules, grinding, adding 15-25ml of methanol, carrying out ultrasonic treatment for 25-35min, filtering, evaporating filtrate to dryness, adding 15-25ml of water for dissolving, adjusting pH to 2-4 with hydrochloric acid, extracting with ethyl acetate for 3 times, 15-25ml each time, combining ethyl acetate solutions obtained by extracting for 3 times, evaporating to dryness, adding 0.5-1.5ml of absolute ethyl alcohol for dissolving to obtain a sample solution; adding methanol into salvianolic acid B to obtain 1-2mg/ml salvianolic acid B solution as reference solution, performing thin layer chromatography, sucking 2-4 μ l sample solution and 1-3 μ l reference solution, and respectively dropping on the same silica gel GF
254Developing the liquid to be detected by using a second developing agent on the thin-layer plate, taking out, airing, and placing under an ultraviolet lamp for inspection, wherein fluorescent spots with the same color appear in the chromatogram of the test sample at the positions corresponding to the chromatograms of the reference sample;
3) detecting the content of emodin and chrysophanol:
(1) liquid chromatography conditions: the chromatographic conditions for determining emodin and chrysophanol are that octadecylsilane chemically bonded silica is used as filler; methanol-phosphoric acid with the concentration of 0.08-0.12% is used as a mobile phase according to the volume ratio of 90: 10; the detection wavelength is 254 +/-2 nm; the flow rate is 1.0 ml/min; column temperature: 25 ℃;
the theoretical plate number is determined according to the following steps: under the test conditions, the theoretical plate number is specified to be 2000-5000 in the system applicability test;
(2) preparation of control solutions: accurately weighing appropriate amount of emodin and chrysophanol reference substances, dissolving with methanol to obtain mixed solution containing emodin 5.46 μ g and chrysophanol 0.992 μ g per 1ml, and storing in dark place;
(3) preparation of a test solution: precisely weighing 1g of liver essence particles, placing in an erlenmeyer flask, precisely adding 45-55ml of methanol, weighing, heating and refluxing for 25-35min, cooling, weighing again, complementing the weight loss with methanol, shaking, filtering, precisely taking 4.8-5.2ml of subsequent filtrate, placing in a 50ml round-bottomed flask, volatilizing ethanol, adding 10ml of 2.5mol/L sulfuric acid solution, ultrasonically treating for 4-6min, adding 10ml of chloroform, heating and refluxing for 55-65min, cooling, transferring to a separating funnel, washing the container with a small amount of chloroform, adding into the separating funnel, separating a chloroform layer, extracting acid solution with chloroform for 2 times, 9-11ml each time, combining the chloroform solution, dehydrating with anhydrous sodium sulfate, transferring the chloroform solution to a 100ml erlenmeyer flask, volatilizing chloroform, precisely adding 8-12ml of methanol into the residue, weighing, placing in a water bath, slightly heating and dissolving the residue, cooling, weighing, adding methanol to make up the lost weight, shaking, filtering the supernatant with 0.45 μm microporous membrane, and collecting the filtrate;
(4) the determination method comprises the following steps: precisely sucking 10 μ l of each of the reference solution and the sample solution, injecting into liquid chromatograph, and measuring.
2. The quality control method of liver-nourishing granules according to claim 1, wherein: in the step 1), the first developing agent used in the development is a mixture of chloroform-acetone-formic acid-water according to a volume ratio of 3-5:4:0.4-0.6: 0.1-0.3.
3. The quality control method of liver-nourishing granules according to claim 1, wherein: in the step 1), the unfolding distance is 8-15 cm during unfolding.
4. The quality control method of liver-nourishing granules according to claim 1, wherein: in the step 2), the second developing agent used in the development is a mixture of toluene-ethyl acetate-formic acid according to a volume ratio of 1.8-2.2:5.8-6.2: 0.8-1.2.
5. The quality control method of liver-nourishing granules according to claim 1, wherein: in the step 2), the unfolding distance is 8-15 cm during unfolding.
6. The quality control method of liver-nourishing granules according to claim 1, wherein: the wavelengths of the ultraviolet lamps used in the step 1) and the step 2) are 254 +/-2 nm.
7. The quality control method of liver-nourishing granules according to claim 1, wherein: the power in the ultrasonic treatment in the step 1) and the step 2) is 50W, and the frequency is 45-60 kHz.
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Application publication date: 20200211 |