CN102435693B - Method for controlling quality of midbody during preparation process of Shenmai injection - Google Patents
Method for controlling quality of midbody during preparation process of Shenmai injection Download PDFInfo
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- CN102435693B CN102435693B CN 201110455674 CN201110455674A CN102435693B CN 102435693 B CN102435693 B CN 102435693B CN 201110455674 CN201110455674 CN 201110455674 CN 201110455674 A CN201110455674 A CN 201110455674A CN 102435693 B CN102435693 B CN 102435693B
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Abstract
The invention relates to a method for controlling the quality of a midbody during a preparation process of a Shenmai injection. The midbody during the preparation process of the Shenmai injection comprises a red ginseng alcohol extract, a red ginseng refined filtrate, a radix ophiopogonis alcohol extract and a radix ophiopogonis refined filtrate, wherein the total weight percent of the solid in the red ginseng alcohol extract is 10.0%-27.0%; counted by the weight of crude drugs, the red ginseng alcohol extract contains 1.06-2.53mg/g of ginsenoside Rg1(C42H72O14) and 0.66-1.42mg/g of ginsenoside Re(C48H82O18); the total weight percent of the solid in the red ginseng refined filtrate is 8.0%-23.0%; counted by the weight of crude drugs, the red ginseng refined filtrate contains 1.06-2.53mg/g of ginsenoside Rg1(C42H72O14) and 0.66-1.42mg/g of ginsenoside Re(C48H82O18); the total weight percent of the solid in the radix ophiopogonis alcohol extract is 8.0%-19.0%; counted by the weight of a dry product and counted by the weight of radix ophiopogonis saponin D(C44H70O16), the total content of the saponin in the radix ophiopogonis alcohol extract is not less than 1.0%; and the total weight percent of the solid in the radix ophiopogonis refined filtrate is 8.0%-19.0%. A purpose of fully controlling the quality of an end product is achieved by controlling the quality of the midbody during the preparation process of the Shenmai injection.
Description
Technical field
The present invention relates to a kind of method of controlling the intermediate quality in the Shenmai injection preparation process.
Background technology
Shenmai injection is mainly used in supplementing QI to prevent collapse, and nourishing Yin and promoting production of body fluid is given birth to arteries and veins.The shock, coronary heart disease, vital myocarditis, chronic cardiopulmonary disease, the agranulocytosis that are used for the treatment of type of deficiency of both QI and YIN.Can improve the immunity function of tumour patient, when share with chemotherapeutics, certain synergistic effect be arranged, and can reduce the caused toxicity of chemotherapeutics.Composition: red ginseng, the tuber of dwarf lilyturf.Auxiliary material is polyoxyethylene sorbitan monoleate, sodium bisulfite.
Proterties: this product is that little yellow is to amber clear liquid.Usage and dosage: intramuscular injection, a 2-4ml, 1 time on the one.Drip-feed, 20-100ml (with using after the 5% glucose injection 250-500ml dilution) or follow the doctor's advice.The national drug standards: WS3-B-3428-98-2010Z.The quality standard of only having finished product in the drug standards can't guarantee the quality control in the preparation process.
Summary of the invention
Technical scheme of the present invention has provided a kind of method of controlling the intermediate quality in the Shenmai injection preparation process.
The invention provides a kind of method of controlling the intermediate quality in the Shenmai injection preparation process, the intermediate in the described Shenmai injection preparation process comprises smart filtrate of the smart filtrate of red ginseng alcohol extract, red ginseng, tuber of dwarf lilyturf alcohol extract, the tuber of dwarf lilyturf; Alcohol extract is as the product of First operation in the technique, and its quality control is particularly crucial; Last procedure before smart filtrate is mixed with as parenteral solution can either be verified the stability that alcohol extract is controlled, and also can further ensure end product quality.
The total solid percentage composition is 10.0%-27.0% in the red ginseng alcohol extract; The red ginseng alcohol extract contains the ginsenoside Rg by the crude drug amount
1(C
42H
72O
14) should be 1.06-2.53mg/g, ginsenoside Re (C
48H
82O
18) should be 0.66-1.42mg/g; The smart filtrate total solid of red ginseng percentage composition is 8.0%-23.0%; The smart filtrate this product of red ginseng contains the ginsenoside Rg by the crude drug amount
1(C
42H
72O
14) 1.06-2.53mg/g, ginsenoside Re (C
48H
82O
18) should be 0.66-1.42mg/g;
The tuber of dwarf lilyturf, alcohol extract total solid percentage composition was 8.0%-19.0%; The tuber of dwarf lilyturf, the alcohol extract total saponin content calculated with dry product, with ophiopogonin D (C
44H
70O
16) meter, be not less than 1.0%; The tuber of dwarf lilyturf, smart filtrate total solid percentage composition was 8.0%-19.0%.
Wherein, the chromatographic condition of described red ginseng alcohol extract finger-print and assay is: chromatographic column: Waters symmetryshield
TMRP
18(4.6mm * 250mm; 5.0 μ m); Column temperature: 30 ℃; Detect wavelength: 203nm; Mobile phase: acetonitrile-water, according to the form below carries out gradient elution; Number of theoretical plate is pressed ginsenoside Rb
1The peak calculates should be not less than 2000000:
The preparation of object of reference solution: precision takes by weighing through ginsenoside Rb
1Reference substance is an amount of, adds 5% methyl alcohol and makes the solution that every 1ml contains 0.2mg, and get final product; The preparation of need testing solution: getting this product, an amount of (about 4～6ml), evaporate to dryness in water-bath, residue add water makes dissolving, put in the 10ml measuring bottle, thin up shakes up to scale (being equivalent to approximately medicinal material 0.1mg/ml), filter with 0.45 μ m miillpore filter, get filtrate, and get final product; Determination method: precision is drawn object of reference solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured.
Described tuber of dwarf lilyturf, the alcohol extract content assaying method was:
Color condition: take perchloric acid as developer;
Reference substance solution: precision takes by weighing ophiopogonin D 5mg, places the 25ml measuring bottle, with methyl alcohol dissolving and be settled to 25ml, and get final product;
The preparation of typical curve: precision is measured reference substance solution 0.1,0.3,0.5,1.0,1.5,2.0ml and is placed respectively the dry tool plug of 10ml test tube, volatilize solvent, the accurate perchloric acid 10ml that adds, reaction is 15 minutes in 65 ℃ of water-baths, cools off with ice-water bath, the retinue solvent is blank, according to UV-VIS spectrophotometry (Chinese Pharmacopoeia version appendix in 2005 V A), measure absorption value in 396nm, take absorption value as ordinate, concentration is horizontal ordinate, the drawing standard curve;
Determination method: precision is measured need testing solution 0.5ml, puts the dry tool plug of 10ml test tube, and method under the sighting target directrix curve item from " volatilizing solvent ", is measured absorbance in accordance with the law, from the amount that typical curve is read ophiopogonin D the need testing solution, calculates, and get final product.
By the quality of the intermediate in the control Shenmai injection preparation process, reach the purpose of comprehensive control finished product quality.
Description of drawings
Fig. 1 joins wheat extract preparation technology process flow diagram and sees
The test sample finger-print of Fig. 2 red ginseng alcohol extract
Fig. 3 red ginseng alcohol extract withinday precision is investigated the result
The result is investigated in the test of Fig. 4 reappearance
Embodiment
Ginseng wheat extract preparation technology process flow diagram is seen Fig. 1
Table 1 injection containing ginseng extract liquid preparing process of the present invention critical process and parameter control criterion
The ginseng ginseng is extracted quality of intermediate amount standard in embodiment 1 Shenmai injection of the present invention
Table 2 red ginseng extracts quality of intermediate amount control project
One, the quality standard of red ginseng alcohol extract
A. proterties this product is yellow to the yellowish-brown clear liquid
The measurement result of table 3 proterties
| The sample lot number | Color proterties (n=3) | Clarity (n=3) |
| 091114-CT | Yellow | Clarification is without muddy |
| 091210-CT | Yellow | Clarification is without muddy |
| 091211-CT | Yellow | Clarification is without muddy |
According to the above results, set the proterties of this product.Consider visual inspection, be set as and be yellow to yellowish-brown.
B. the total solid precision is got this product 10ml and is put in the constant weight evaporating dish, behind evaporate to dryness in the water-bath 105 ℃ of dryings 3 hours to constant weight, the total cooling of dislocation exsiccator 30 minutes, weighed weight, calculate the content of solid content, and be converted into the percentage composition of weight (mg/g) according to the crude drug amount.The results are shown in Table 4.
Table 4 red ginseng alcohol extract total solids content measured value (%)
With each batch measured value ± 20% upper and lower limit that settles the standard, working out limit is 10.0%-27.0%.After having accumulated aborning more data from now on, revise again more suitably limit.
C. finger-print
This test is mainly done the precision that detects and reappearance and is checked, and sets up red ginseng alcohol extract internal control finger-print standard.
C.1 instrument and reagent
Agilent 1100 series of high efficiency liquid chromatographs (Chemstation chromatographic work station), Mettler AE240 electronic balance, acetonitrile and methyl alcohol are chromatographically pure, and water is double distilled water, and it is pure that all the other reagent are analysis.
C.2 chromatographic condition:
Chromatographic column: Waters symmetryshield
TMRP
18(4.6mm * 250mm; 5.0 μ m);
Column temperature: 30 ℃
Detect wavelength: 203nm
Mobile phase: acetonitrile-water, according to the form below carries out gradient elution; Number of theoretical plate is pressed ginsenoside Rb
1The peak calculates should be not less than 2000000.
Integral parameter: Slope Sensitivity:5, peak width:0.05, smallest peaks area are 10% of S peak-to-peak area; Minimum peak height be the S peak-to-peak high 10%, the baseline integration, limit of integration is 5～105 minutes.
The preparation of object of reference solution: precision takes by weighing through ginsenoside Rb
1Reference substance is an amount of, adds 5% methyl alcohol and makes the solution that every 1ml contains 0.2mg, and get final product.
The preparation of need testing solution: getting this product, an amount of (about 4～6ml), evaporate to dryness in water-bath, residue add water makes dissolving, put in the 10ml measuring bottle, thin up shakes up to scale (being equivalent to approximately medicinal material 0.1mg/ml), filter with 0.45 μ m miillpore filter, get filtrate, and get final product.
Determination method: precision is drawn object of reference solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured.(seeing Fig. 2)
C.3 precision test is got red ginseng alcohol extract (lot number: 091210-CT) make need testing solution, draw respectively each 10 μ l injection liquid chromatography of reference substance and need testing solution, measure by above-mentioned chromatographic condition, and get final product.Test sample continuous sample introduction 5 pins wherein.Select first 16 chromatographic peaks as total chromatographic peak, calculate relative peak area, see Table 5, Fig. 3:
Therefore the RSD value of relative peak area less than 3.0%, illustrates that the withinday precision test findings of red ginseng alcohol extract finger-print is good 0.22%～2.63%.
C.4 the reappearance test is got red ginseng alcohol and is got extract (lot number: 091210) 4.5ml, 5 parts of the same form, respectively at evaporate to dryness in the water-bath, residue adds water makes dissolving, puts in the 10ml measuring bottle, thin up is to scale, shake up, filter with 0.45 μ m miillpore filter, get filtrate 10 μ l injection liquid chromatographies, measure by above-mentioned chromatographic condition, and get final product.Select first 15 chromatographic peaks as total chromatographic peak, calculate relative peak area, see Table 6, Fig. 4:
Therefore the RSD value of relative peak area less than 3.0%, illustrates that the withinday precision test findings of red ginseng alcohol extract finger-print is good 0.18%～2.65%.
C.5 red ginseng alcohol extract standard control finger-print inner quality standard is set up
This product finger-print as calculated machine simulation similarity software (similarity evaluation version in 2004) B version calculates
D. assay
The preparation of instrument and reagent, chromatographic condition, need testing solution is same C.1, C.2, and theoretical cam curve is calculated by the ginsenoside Re should be not less than 300000, the ginsenoside Rg
1Must not be lower than 1.8. with the degree of separation of Re
The preparation of reference substance solution: precision takes by weighing the ginsenoside Rg
1An amount of with the Re reference substance, add 5% methyl alcohol and make the solution that every 1ml contains respectively 0.1mg and 0.08mg.
D.1 precision test
Adopt a D.3 lower method mensuration, wherein need testing solution continuous sample introduction 6 pins calculate the ginsenoside Rg
1Content with Re.Experimental result sees Table 7.
Table 7 Precision test result
Result: ginsenoside Rg
1Peak area RSD%=0.56%, ginsenoside Re's peak area RSD%=0.96% all less than 1.5%, shows that this content assaying method precision is good.
D.2 reappearance test
Adopt a C.4 lower method mensuration, get respectively reference substance solution and need testing solution sample introduction and measure, calculate the ginsenoside Rg
1Content with Re.Experimental result sees Table 8.
Table 8 reproducible test results
Result: ginsenoside Rg
1Peak area RSD%=0.10%, ginsenoside Re's peak area RSD%=0.74% all less than 1.5%, shows that this content assaying method reappearance is good.
D.3 red ginseng alcohol extract sample determination
Measure ginsenoside Rg in 3 batches of red ginseng alcohol extracts
1With ginsenoside Re's content, and press the crude drug amount and convert the ginsenoside Rg
1Content range is at 1.37～2.11mg/g, and ginsenoside Re's content range is at 0.83～1.18mg/g.Consider the diversity of crude drug source, by minimum mxm. ± 20% determine the content bound, determine that this product by the crude drug amount, contains the ginsenoside Rg
1(C
42H
72O
14) should be 1.06-2.53mg/g, ginsenoside Re (C
48H
82O
18) should be 0.66-1.42mg/g.The results are shown in Table 9.
Table 9 red ginseng alcohol extract sample determination result
| The sample lot number | The ginsenoside Rg1 | The ginsenoside Re |
| 091114-CT | 2.11 | 1.18 |
| 091210-CT | 1.37 | 0.83 |
| 091211-CT | 1.39 | 0.88 |
| Mean value | 1.62 | 0.96 |
Two, the smart filtrate standard of red ginseng
A, proterties this product are yellow to the yellowish-brown clear liquid
The measurement result of proterties
| The sample lot number | Color proterties (n=3) | Clarity (n=3) |
| 091114-J | Yellow | Clarification is without muddy |
| 091210-J-1 | Yellow | Clarification is without muddy |
| 091210-J-2 | Yellow | Clarification is without muddy |
| 091211-J-1 | Yellow | Clarification is without muddy |
| 091211-J-2 | Yellow | Clarification is without muddy |
According to the above results, set the proterties of this product.Consider visual inspection, be set as and be yellow to yellowish-brown.
B, pH value
B.1 instrument: PHS-3C acidometer
B.2 measurement result:
The smart filtrate pH of table 10 red ginseng pH-value determination pH result
According to measurement result, determine that the pH value should be 6.5～8.5.
C, total solid precision are got this product 10ml and are put in the constant weight evaporating dish, behind evaporate to dryness in the water-bath 105 ℃ of dryings 3 hours to constant weight, the total cooling of dislocation exsiccator 30 minutes, weighed weight, calculate the content of solid content, and be converted into the percentage composition of weight according to the crude drug amount.The results are shown in Table 11.
The smart filtrate total solids content measured value (%) of table 11 red ginseng
By actual measurement sample minimum mxm. ± 20% determine the total solid bound, working out limit is 8.0%-23.0%.Accumulated aborning from now on after many data, revised again more suitably limit.
D. finger-print
Adopt red ginseng alcohol extract fingerprint spectrum method, see red ginseng alcohol extract inner quality standard for details.
D.1 the smart filtrate standard control of red ginseng finger-print inner quality standard is set up
This product finger-print as calculated machine simulation similarity software (similarity evaluation version in 2004) B version calculates.
E, assay
E.1 adopt red ginseng alcohol extract content assaying method, see red ginseng alcohol extract standard for details.
E.2 C.1 instrument and reagent, chromatographic condition draft, C.2 with red ginseng alcohol extract standard, and theoretical cam curve is calculated by the ginsenoside Re should be not less than 300000, the ginsenoside Rg
1Must not be lower than 1.8 with the degree of separation of Re.
The preparation of need testing solution: getting this product, an amount of (about 1.5～3ml), evaporate to dryness in water-bath, residue add water makes dissolving, put in the 10ml measuring bottle, thin up shakes up to scale (being equivalent to approximately medicinal material 0.1mg/ml), filter with 0.45 μ m miillpore filter, get filtrate, and get final product.
The preparation of reference substance solution: precision takes by weighing the ginsenoside Rg
1An amount of with the Re reference substance, add 5% methyl alcohol and make the solution that every 1ml contains respectively 0.1mg and 0.08mg.
E.3 the smart filtrate sample of red ginseng is measured
Measure ginsenoside Rg in the smart filtrate of 5 batches of red ginsengs
1With ginsenoside Re's content, and press the crude drug amount and convert the ginsenoside Rg
1Content range is at 1.36-2.05mg/g, and ginsenoside Re's content range is at 0.84-1.15mg/g.Consider the diversity of crude drug source, determine that this product by the crude drug amount, contains the ginsenoside Rg
1(C
42H
72O
14) 1.06-2.53mg/g, ginsenoside Re (C
48H
82O
18) should be 0.66-1.42mg/g.The results are shown in Table 12.
The smart filtrate sample measurement result of table 12 red ginseng
| The sample lot number | The ginsenoside Rg1 | The ginsenoside Re |
| 091114-J | 2.05 | 1.15 |
| 091210-J-1 | 1.41 | 0.84 |
| 091210-J-2 | 1.74 | 1.05 |
| 091211-J-1 | 1.36 | 0.84 |
| 091211-J-2 | 1.45 | 0.89 |
| Mean value | 1.60 | 0.95 |
Embodiment 2 Shenmai injection ophiopogon japonicus extract quality standards of the present invention
Table 13 extracts quality of intermediate amount control project the tuber of dwarf lilyturf
One, the tuber of dwarf lilyturf, the alcohol extract standard was drafted explanation
A, proterties this product are that little yellow refers to yellow clear liquid.
The measurement result of table 14 proterties
| The sample lot number | Color proterties (n=3) | Clarity (n=3) |
| C091101CT | Little yellow | Clarification |
| 091204CT | Little yellow | Clarification |
According to the above results, set the proterties of this product.Consider visual inspection, be set as and be little yellow～yellow.
B, total solid precision are got this product 10ml and are put in the constant weight evaporating dish, behind evaporate to dryness in the water-bath 105 ℃ of dryings 3 hours to constant weight, the total cooling of dislocation exsiccator 30 minutes, weighed weight, calculate the content of solid content, and be converted into the percentage composition of mg/g according to the crude drug amount.The results are shown in Table 15.
Table 15 alcohol extract tuber of dwarf lilyturf total solids content measured value (%)
Working out limit is 8.0%-19.0%.
C, assay
Be the control extraction quality of the tuber of dwarf lilyturf, we are chosen in tuber of dwarf lilyturf alcohol extract and measure its total saponin content.Total saponin(e assay method specificity of recording in the Shenmai injection finished product standard is relatively poor, and precision and the reappearance of sample determination are bad.The present invention has set up take ophiopogonin D as reference substance, the content method of the total saponin(e of the determined by ultraviolet spectrophotometry alcohol extract tuber of dwarf lilyturf.
C.1 instrument and reagent
Shimadzu UV-2100 ultraviolet spectrophotometer (Shimadzu Corp), the Mettler electronic balance.Ophiopogonin D reference substance (the Chengdu Cisco China HPLC of Bioisystech Co., Ltd 〉=98.0%), perchloric acid, anhydrous dextrose, methyl alcohol are that analysis is pure, experimental water is purified water.
C.2 color condition is take perchloric acid as developer
C.3 the selection of absorbing wavelength
C.4 the reference substance solution precision takes by weighing ophiopogonin D 5mg, places the 25ml measuring bottle, with methyl alcohol dissolving and be settled to 25ml, and get final product.
C.5 the preparation of typical curve
Precision is measured reference substance solution 0.1,0.3,0.5,1.0,1.5,2.0ml and is placed respectively the dry tool plug of 10ml test tube, volatilize solvent, the accurate perchloric acid 10ml that adds, reaction is 15 minutes in 65 ℃ of water-baths, cools off with ice-water bath, the retinue solvent is blank, according to UV-VIS spectrophotometry (Chinese Pharmacopoeia version appendix in 2005 V A), measure absorption value in 396nm, take absorption value as ordinate, concentration is horizontal ordinate, the drawing standard curve.
The determination method precision is measured need testing solution 0.5ml, puts the dry tool plug of 10ml test tube, and method under the sighting target directrix curve item from " volatilizing solvent ", is measured absorbance in accordance with the law, from the amount that typical curve is read ophiopogonin D the need testing solution, calculates, and get final product.
C.6 application of sample recovery experiment precision is measured alcohol extracting tuber of dwarf lilyturf need testing solution (C091101-CT) 0.5ml, puts the dry tool plug of 10ml test tube, and totally 9 parts, precision adds ophiopogonin D reference substance solution 0.2,0.5,1.0ml respectively again, each three parts of each concentration; Retinue get with batch tuber of dwarf lilyturf alcohol extract 0.5ml compare.Method under the sighting target directrix curve item from " volatilizing solvent ", is measured absorbance in accordance with the law, reads the amount that application of sample reclaims ophiopogonin D each sample from typical curve, tries to achieve the ophiopogonin D recovery, the results are shown in Table 16.
Table 16 alcohol extract tuber of dwarf lilyturf assay application of sample recovery experiment result
The application of sample recovery test is the result show: because of spectrophotometric method method limitation, accuracy is not high enough, and average recovery rate is 91.3%, but variation is less, and the recovery of high, medium and low concentration is all more stable, the reference method of the content control of product in the middle of therefore can be used as.
C.7 reappearance test precision is got alcohol extracting tuber of dwarf lilyturf need testing solution (C091101-CT) 0.5ml, totally 5 parts, put the dry tool plug of 10ml test tube, method under the sighting target directrix curve item, from " volatilizing solvent ", measure absorbance in accordance with the law, from the amount that typical curve is read ophiopogonin D the need testing solution, calculate total saponin content and RSD value in the alcohol extract tuber of dwarf lilyturf.(seeing Table 17)
Table 17 alcohol extract tuber of dwarf lilyturf total saponin content assay method reproducible test results
The method reappearance is good.
C.8 arbitrary duplicate samples in the reappearance test is got in stability test, and timing after finishing with chromogenic reaction is measured absorption value in 396nm, records 0,30,60,90,120,180 minute absorption value (seeing Table 18)
Table 18 content assaying method tuber of dwarf lilyturf stability test result
As seen: after the tuber of dwarf lilyturf, the herbal extract chromogenic reaction stopped, should in 60 minutes, measure absorbance log.
C.9 the many batches of alcohol extract total saponin content measurement results tuber of dwarf lilyturf (seeing Table 19)
Table 19 different batches alcohol extract tuber of dwarf lilyturf assay result
| Lot number | Total saponin content (g/g) |
| C091101CT | 1.52％ |
| 091204CT | 1.51％ |
Just build because of alcohol extracting tuber of dwarf lilyturf total saponin content assay method, data accumulation is few, thus determine the inner quality standard lower limit with-30% of mean value, wouldn't capping.Be the tuber of dwarf lilyturf alcohol extract total saponin content calculate with dry product, with ophiopogonin D (C
44H
70O
16) meter, be not less than 1.0%.
Two, the tuber of dwarf lilyturf, smart filtrate standard was drafted explanation
A, the little yellow of proterties this product refer to yellow clear liquid.
The measurement result of table 20 proterties
| The sample lot number | Color proterties (n=3) | Clarity (n=3) |
| C091101-1-J | Little yellow | Clarification |
| C091101-2-J-1 | Little yellow | Clarification |
| C091101-2-J-2 | Little yellow | Clarification |
| 091204-J-1 | Little yellow | Clarification |
| 091204-J-2 | Little yellow | Clarification |
B, pH value
B.1 instrument: PHS-3C acidometer
B.2 measurement result:
Table 21 smart filtrate pH tuber of dwarf lilyturf pH-value determination pH result
According to measurement result, determine that the pH value should be 6.0～7.0
C, total solid precision are got this product 10ml and are put in the constant weight evaporating dish, behind evaporate to dryness in the water-bath 105 ℃ of dryings 3 hours to constant weight, the total cooling of dislocation exsiccator 30 minutes, weighed weight, calculate the content of solid content, and be converted into the percentage composition of weight (mg/g) according to the crude drug amount.The results are shown in Table 22.
Table 22 smart filtrate total solids content measured value (%) tuber of dwarf lilyturf
Working out limit is 8.0%-19.0%, accumulated aborning more data from now on after, revise again more suitably limit.
For guaranteeing the stable of production run, because may there be certain error in metering method, intermediate has been stipulated following normal fluctuation range simultaneously in addition.(take every crowd of dosing amount 1200L as example)
Table 23 red ginseng intermediate volume term of reference and crude drug content
Table 24 intermediate tuber of dwarf lilyturf volume term of reference and crude drug content
Table 25 Quality control of intermediates project
Claims (1)
1. method that detects the intermediate quality in the Shenmai injection preparation process is characterized in that: the intermediate in the described Shenmai injection preparation process comprises smart filtrate of red ginseng alcohol extract, the smart filtrate of red ginseng, tuber of dwarf lilyturf alcohol extract, the tuber of dwarf lilyturf;
The total solid percentage composition is 10.0%-27.0% in the red ginseng alcohol extract; The red ginseng alcohol extract contains the ginsenoside Rg by the crude drug amount
1C
42H
72O
14Should be 1.06-2.53 mg/g, ginsenoside Re C
48H
82O
18Should be 0.66-1.42 mg/g; The smart filtrate total solid of red ginseng percentage composition is 8.0%-23.0%; The smart filtrate this product of red ginseng contains the ginsenoside Rg by the crude drug amount
1C
42H
72O
141.06-2.53 mg/g, ginsenoside Re C
48H
82O
18Should be 0.66-1.42 mg/g;
The tuber of dwarf lilyturf, alcohol extract total solid percentage composition was 8.0%-19.0%; The tuber of dwarf lilyturf, the alcohol extract total saponin content calculated with dry product, with ophiopogonin D C
44H
70O
16Meter is not less than 1.0%; The tuber of dwarf lilyturf, smart filtrate total solid percentage composition was 8.0%-19.0%;
Wherein, the chromatographic condition of red ginseng alcohol extract finger-print and assay is:
Chromatographic column: Waters symmetryshield
TMRP
184.6mm * 250mm; 5.0 μ m; Column temperature: 30 ℃; Detect wavelength: 203nm; Mobile phase: acetonitrile-water, according to the form below carries out gradient elution; Number of theoretical plate is pressed ginsenoside Rb
1The peak calculates should be not less than 2000000:
The preparation of object of reference solution: precision takes by weighing through ginsenoside Rb
1Reference substance is an amount of, adds 5% methyl alcohol and makes the solution that every 1ml contains 0.2mg, and get final product; The preparation of need testing solution: get this product 4～6ml, evaporate to dryness in water-bath, residue add water makes dissolving, puts in the 10ml measuring bottle, and thin up is equivalent to medicinal material 0.1mg/ml to scale, shakes up, and filters with 0.45 μ m miillpore filter, gets filtrate, and get final product; Determination method: precision is drawn object of reference solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured;
Described tuber of dwarf lilyturf, the alcohol extract content assaying method was:
Color condition: take perchloric acid as developer;
Reference substance solution: precision takes by weighing ophiopogonin D 5mg, places 25 ml measuring bottles, with methyl alcohol dissolving and be settled to 25 ml, and get final product;
The preparation of typical curve: precision is measured reference substance solution 0.1,0.3,0.5,1.0,1.5,2.0 ml place respectively the dry tool plug of 10 ml test tube, volatilize solvent, the accurate perchloric acid 10ml that adds, reaction is 15 minutes in 65 ℃ of water-baths, cools off with ice-water bath, the retinue solvent is blank, according to the described UV-VIS spectrophotometry of Chinese Pharmacopoeia version appendix in 2005 V A, measure absorption value in 396nm, take absorption value as ordinate, concentration is horizontal ordinate, the drawing standard curve;
Determination method: precision is measured need testing solution 0.5 ml, puts the dry tool plug of 10 ml test tube, and method under the sighting target directrix curve item from " volatilizing solvent ", is measured absorbance in accordance with the law, from the amount that typical curve is read ophiopogonin D the need testing solution, calculates, and get final product.
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| 制备工艺对参麦注射液质量的影响;吴永江;《中国中药杂志》;20050531;第30卷(第9期);第662-665页 * |
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