CN101013110B - Quality controlling method of Bupleurum injection - Google Patents
Quality controlling method of Bupleurum injection Download PDFInfo
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Abstract
The invention discloses Bupleurum injection quality control method. Bupleurum injection quality control method of this invention includes the following steps: the first step, using gas chromatography to establish Bupleurum injection comparison fingerprint pattern: the second step, according to the first step, measuring Bupleurum injection testing saple fingerprint pattern; the third step, calculating similarity of Bupleurum injection testing sample fingerprint pattern and comparison fingerprint pattern, and screening the samples according with Bupleurum injection fingerprint pattern detection standard as qualified products. Through the establishment of Bupleurum injection fingerprint pattern, the invention uses fingerprint pattern to control the quality of Bupleurum injection, with advantages of good repeatability, higher stability, and so on, and it can effectively monitor the quality of Bupleurum injection, to ensure stable and consistent Bupleurum injection clinical effect, and it has important application value.
Description
Technical field
The present invention relates to the method for quality control of Bupleurum injection, particularly relate to the method that employing fingerprint collection of illustrative plates is controlled Bupleurum injection quality.
Background technology
Bupleurum injection is the traditional Chinese medicine injection of early developing, and has the effect of relieving superficies by cooling, is used for the treatment of in a large number the heatings such as flu, influenza and malaria, has definite curative effect.At present, for the method for quality control of Bupleurum injection, be mainly to check absorbance log and pH value, absorbance log: precision measures parenteral solution 5ml, puts in 50ml measuring bottle, is diluted with water to scale, shakes up, as need testing solution.Another precision measures parenteral solution 5ml, puts in evaporating dish, and evaporate to dryness in water-bath, adds water and make to dissolve, and moves in 50ml measuring bottle, is diluted with water to scale, shakes up, as blank.According to spectrophotometric method (< < Drug Standard of Ministry of Public Health of the Peoples Republic of China > > appendix VA), measure, at 278nm and 243nm wavelength place, have respectively absorption maximum and minimal absorption, the absorbance log at 278nm wavelength place is not less than 0.65.PH value: should be 4.0~7.0 (< < Drug Standard of Ministry of Public Health of the Peoples Republic of China > > appendix VII G).But our research shows, the detection of this detection method medium ultraviolet absorbance log is actually the reflection of toxic ingredient furfural, and this detection method is differentiated without specificity and the more effective method of quality control such as assay; In addition parenteral solution is used be Radix Bupleuri through the aqua aromatica of distillation gained, mainly, containing volatile ingredient, its quality is more unstable, has had a strong impact on clinical efficacy and the security of this medicine.
Summary of the invention
The method of quality control that the object of this invention is to provide a kind of Bupleurum injection, particularly utilizes the finger-print of Bupleurum injection to carry out the method for quality control of Bupleurum injection.
The method of quality control of Bupleurum injection of the present invention, comprises the steps:
The first step, vapor-phase chromatography is set up Bupleurum injection reference fingerprint: adopt nonpolar or low pole quartz capillary column, with N
2for carrier gas, flow velocity 0.8-1.5mL/min, current constant mode, split ratio is 10-20: 1; Take FID as detecting device, adopt the mode of temperature programme to analyze; Need testing solution injecting chromatograph by least 10 batches of Bupleurum injections, records chromatogram, utilizes fingerprint similarity evaluation software to generate Bupleurum injection reference fingerprint;
Second step, measures by the first step method finger-print that Bupleurum injection detects sample;
The 3rd step, calculates Bupleurum injection and detects the finger-print of sample and the similarity of reference fingerprint, and similarity is greater than more than 0.7 specification product that are.
In above-mentioned steps 1) while setting up Bupleurum injection reference fingerprint, generally choose the Radix Bupleuri in the genuine place of production and make Bupleurum injection according to following step:
Get the genuine Radix Bupleuri 1000g (place of production: Hebei, Shanxi, Shaanxi, Gansu) that is no more than half a year storage period, be cut into a cun section, rinse well, add the purified water of 11 times of amounts, 70 ℃ of temperature are soaked 8 hours.Through steam distillation, collect just distillate of 6000mL, then re-distillation, collect double distilled liquid, about 1000mL.Add 3.0g Tween-80, stir oil is dissolved completely, then add 9.0g sodium chloride, after dissolving, filter, inject water to 1000mL, with 10% sodium hydroxide solution, regulate pH value to 7.0, with 0.45 μ m miillpore filter, filter, embedding, 100 ℃ of sterilizings 30 minutes, obtain Bupleurum injection.Then according to the preparation method of Bupleurum injection need testing solution, prepare need testing solution.
Wherein, the finger-print of gained of the present invention as shown in Figure 2, valeral peak be take as reference in each total peak, calculate relative retention time (relative retention time ± SD) as follows with relative peak area (the relative peak area ± SD that retains): No. 1 peak relative retention time is 0.500 ± 0.001, relative peak area 45.673 ± 100.619; No. 2 peak relative retention time is 0.527 ± 0.001, and relative peak area is 98.828 ± 343.681; No. 3 peak relative retention time is 0.553 ± 0.002, and relative peak area is 1.308 ± 1.898; No. 4 peak relative retention time is 0.677 ± 0.002, and relative peak area is 0.320 ± 0.229; No. 5 peak relative retention time is 0.838 ± 0.004, and relative peak area is 0.285 ± 0.293; No. 6 peak is 1.000 ± 0.000, and relative peak area is 1.000 ± 0.000; No. 7 peak relative retention time is 1.467 ± 0.006, and relative peak area is 0.386 ± 0.406; No. 8 peak relative retention time is 1.724 ± 0.002, and relative peak area is 1.947 ± 1.498; No. 9 peak relative retention time is 2.040 ± 0.006, and relative peak area is 0.837 ± 1.964; No. 10 peak relative retention time is 2.414 ± 0.008, and relative peak area is 0.697 ± 0.750; No. 11 peak relative retention time is 2.716 ± 0.006, and relative peak area is 0.639 ± 0.431; No. 12 peak relative retention time is 3.335 ± 0.010, and relative peak area is 0.300 ± 0.477; No. 13 peak relative retention time is 3.465 ± 0.011, and relative peak area is 0.241 ± 0.245; No. 14 peak relative retention time is 3.531 ± 0.013, and relative peak area is 0.182 ± 0.357; No. 15 peak relative retention time is 3.695 ± 0.013, and relative peak area is 0.161 ± 0.175; No. 16 peak relative retention time is 3.941 ± 0.018, and relative peak area is 0.149 ± 0.201; No. 17 peak relative retention time is 4.030 ± 0.015, and relative peak area is 0.240 ± 0.299; No. 18 peak relative retention time is 4.105 ± 0.016, and relative peak area is 0.208 ± 0.221.
In the present invention, quartz capillary column is preferably dimethyl siloxane for the fixing quartz capillary column of phase.
FID testing conditions is: injector temperature is 220-250 ℃, and detector temperature is 250-270 ℃.The condition of temperature programme is: initial 35 ℃, keep 2min; 1 ℃/min rises to 40 ℃, keeps 2min, and 3 ℃/min rises to 60 ℃, keeps 3min, and 7 ℃/min rises to 200 ℃, keeps 3min.
The preparation method of need testing solution is: the accurate Bupleurum injection 1.0ml that draws, put in 10ml head space bottle, and seal, obtain need testing solution.Wherein, adopt the condition of headspace sampling mode to be: head space bottle temperature 80-90 ℃, sampling valve temperature 90-120 ℃, transmission line temperature 110-120 ℃; Head space bottle equilibration time 10-25min, head space bottle pressurising time 0.1-0.5min, quantitatively ring filling time 0.1-0.5min, quantitatively encircles equilibration time 0.2-1.0min, sample injection time 0.5-2.0min.
Need testing solution preparation method is except headspace sampling, can also adopt direct injected after organic solvent extraction, concrete operations are: the accurate 10ml Bupleurum injection of drawing, and with heavily steaming ether equivalent extracting twice, each 10ml, combined ether layer, add anhydrous sodium sulfate dehydration 30 minutes, filter, filtrate vacuum is drained, residue is 5ml with heavily steaming ether dissolution constant volume, obtains described need testing solution.
The present invention is by setting up the finger-print of Bupleurum injection, employing fingerprint collection of illustrative plates is controlled the quality of Bupleurum injection, there is reproducible, stability advantages of higher, quality that can effective monitoring Bupleurum injection, can guarantee the stable, consistent of Bupleurum injection clinical efficacy, there is important using value.
Accompanying drawing explanation
Fig. 1 is 10 crowdes of Bupleurum injection sample finger-print stacking diagrams;
Fig. 2 is the reference fingerprint of Bupleurum injection;
Fig. 3 is the finger-print of continuous sample introduction 5 pins of same lot number Bupleurum injection;
Fig. 4 is that same sample solution is respectively at the finger-print of 0,1,2,4,8 hour sample introduction;
Fig. 5 is the finger-print of same lot number repetitive operation 5 times.
Embodiment
The foundation of experimental example 1, Bupleurum injection reference fingerprint
1, the selection of detection method:
Bupleurum injection, mainly containing volatile ingredient, therefore adopts GC-FID method to set up finger-print proper.
2, the investigation of chromatographic column:
Respectively to Agilent HP-5 30m * 0.32mm * 0.25 μ m (low pole); Agilent DB-WAX 30m * 0.53mm * 1 μ m (strong polarity); Three kinds of gas chromatographies of Agilent DB-624 30m * 0.32mm * 1.8 μ m (nonpolar) are investigated, result shows that the HP-5 capillary column separating effect of nonpolar DB-624 and low pole is better, be suitable for the detection of Bupleurum injection finger-print, HP-5 capillary column (dimethyl siloxane as the fixedly phase) separating effect of wherein take is again best.
3, the preparation method of need testing solution:
We have investigated hand sampling after headspace sampling and organic solvent extraction, find that two kinds of modes all can realize the detection of finger-print.
Test sample preparation method:
Organic solvent extractionprocess need testing solution preparation method: get 10 of parenteral solutions, after fully mixing, the accurate 10ml that draws is with heavily steaming ether equivalent extracting twice, each 10ml, combined ether layer, adds anhydrous sodium sulfate dehydration 30 minutes, filters, filtrate vacuum is drained, and residue is that 5ml is standby with heavily steaming ether dissolution constant volume.The accurate 1 μ l sample introduction of drawing.
Headspace sampling need testing solution preparation method: the accurate Bupleurum injection 1.0ml that draws, put in 10ml head space bottle, seal, obtain.
The condition of headspace sampling is: head space bottle temperature 80-90 ℃, sampling valve temperature 90-120 ℃, transmission line temperature 110-120 ℃; Head space bottle equilibration time 10-25min, head space bottle pressurising time 0.1-0.5min, quantitatively ring filling time 0.1-0.5min, quantitatively encircles equilibration time 0.2-1.0min, sample injection time 0.5-2.0min.
4, determination method
By Bupleurum injection test sample, with hand sampling or through head-space sampler sample introduction, inject gas chromatograph, records the chromatogram of 42 minutes.
With N
2for carrier gas, flow velocity 0.8-1.5mL/min, current constant mode, split ratio is 10: 1-20: 1; Take FID as detecting device, and injector temperature is 220-250 ℃, and detector temperature is 250-270 ℃, adopts the mode of temperature programme to analyze, and the optimum condition of temperature programme is: initial 35 ℃, keep 2min; 1 ℃/min rises to 40 ℃, keeps 2min, and 3 ℃/min rises to 60 ℃, keeps 3min, and 7 ℃/min rises to 200 ℃, keeps 3min.
5, the foundation of Bupleurum injection reference fingerprint
The preparation of Bupleurum injection: get the genuine Radix Bupleuri 1000g (place of production: Hebei, Shanxi, Shaanxi, Gansu) that is no more than half a year storage period, be cut into a cun section, rinse well, add the purified water of 11 times of amounts, 70 ℃ of temperature are soaked 8 hours.Through steam distillation, collect just distillate of 6000mL, then re-distillation, collect double distilled liquid, about 1000mL.Add 3.0g Tween-80, stir oil is dissolved completely, then add 9.0g sodium chloride, after dissolving, filter, inject water to 1000mL, with 10% sodium hydroxide solution, regulate pH value to 7.0, with 0.45 μ m miillpore filter, filter, embedding, 100 ℃ of sterilizings 30 minutes, obtain Bupleurum injection.
By the preparation method of Bupleurum injection, prepare the parenteral solution of 10 batches, measure its finger-print, 10 crowdes of Bupleurum injection sample finger-print stacking diagrams are as Fig. 1.Adopt similarity evaluation software to carry out similarity calculating to 10 batches of Bupleurum injection sample finger-prints, the results are shown in Table 1.
The common pattern that utilizes similarity Software Create Bupleurum injection sample finger-print, obtains reference fingerprint, as Fig. 2.Utilize GC-MS to point out the chromatographic peak in Bupleurum injection, each peak ownership is in Table 2.
In Fig. 2, being take in No. 6 peak-valeral peaks at each total peak is reference, calculates relative retention time (relative retention time ± SD) and relative peak area (the relative peak area ± SD that retains):
No. 1 peak relative retention time is 0.500 ± 0.001, relative peak area 45.673 ± 100.619; No. 2 peak relative retention time is 0.527 ± 0.001, and relative peak area is 98.828 ± 343.681; No. 3 peak relative retention time is 0.553 ± 0.002, and relative peak area is 1.308 ± 1.898; No. 4 peak relative retention time is 0.677 ± 0.002, and relative peak area is 0.320 ± 0.229; No. 5 peak relative retention time is 0.838 ± 0.004, and relative peak area is 0.285 ± 0.293; No. 6 peak is 1.000 ± 0.000, and relative peak area is 1.000 ± 0.000; No. 7 peak relative retention time is 1.467 ± 0.006, and relative peak area is 0.386 ± 0.406; No. 8 peak relative retention time is 1.724 ± 0.002, and relative peak area is 1.947 ± 1.498; No. 9 peak relative retention time is 2.040 ± 0.006, and relative peak area is 0.837 ± 1.964; No. 10 peak relative retention time is 2.414 ± 0.008, and relative peak area is 0.697 ± 0.750; No. 11 peak relative retention time is 2.716 ± 0.006, and relative peak area is 0.639 ± 0.431; No. 12 peak relative retention time is 3.335 ± 0.010, and relative peak area is 0.300 ± 0.477; No. 13 peak relative retention time is 3.465 ± 0.011, and relative peak area is 0.241 ± 0.245; No. 14 peak relative retention time is 3.531 ± 0.013, and relative peak area is 0.182 ± 0.357; No. 15 peak relative retention time is 3.695 ± 0.013, and relative peak area is 0.161 ± 0.175; No. 16 peak relative retention time is 3.941 ± 0.018, and relative peak area is 0.149 ± 0.201; No. 17 peak relative retention time is 4.030 ± 0.015, and relative peak area is 0.240 ± 0.299; No. 18 peak relative retention time is 4.105 ± 0.016, and relative peak area is 0.208 ± 0.221.
10 batches of Bupleurum injection sample fingerprint similarity result of calculation tables of table 1
041012 | 041013 | 041014 | 041015 | 041023 | 041024 | 041025 | 041026 | 041027 | 041028 | Reference fingerprint | |
041012 | 1.000 | 0.949 | 0.975 | 0.944 | 0.940 | 0.901 | 0.958 | 0.967 | 0.972 | 0.868 | 0.956 |
041013 | 0.949 | 1.000 | 0.993 | 0.991 | 0.997 | 0.989 | 0.997 | 0.970 | 0.979 | 0.974 | 0.999 |
041014 | 0.975 | 0.993 | 1.000 | 0.992 | 0.985 | 0.968 | 0.992 | 0.984 | 0.989 | 0.943 | 0.995 |
041015 | 0.944 | 0.991 | 0.992 | 1.000 | 0.981 | 0.976 | 0.983 | 0.974 | 0.977 | 0.950 | 0.990 |
041023 | 0.940 | 0.997 | 0.985 | 0.981 | 1.000 | 0.994 | 0.996 | 0.957 | 0.968 | 0.984 | 0.995 |
041024 | 0.901 | 0.989 | 0.968 | 0.976 | 0.994 | 1.000 | 0.985 | 0.936 | 0.947 | 0.993 | 0.985 |
041025 | 0.958 | 0.997 | 0.992 | 0.983 | 0.996 | 0.985 | 1.000 | 0.969 | 0.977 | 0.968 | 0.997 |
041026 | 0.967 | 0.970 | 0.984 | 0.974 | 0.957 | 0.936 | 0.969 | 1.000 | 0.998 | 0.913 | 0.980 |
041027 | 0.972 | 0.979 | 0.989 | 0.977 | 0.968 | 0.947 | 0.977 | 0.998 | 1.000 | 0.928 | 0.987 |
041028 | 0.866 | 0.974 | 0.943 | 0.950 | 0.984 | 0.993 | 0.968 | 0.913 | 0.928 | 1.000 | 0.970 |
Reference fingerprint | 0.956 | 0.999 | 0.995 | 0.990 | 0.995 | 0.985 | 0.997 | 0.980 | 0.987 | 0.970 | 1.000 |
Table 2 Bupleurum injection GC-MS detects ownership table
Peak number | Composition title | Peak number | Composition title |
1 2 3 4 5 6 7 | Propane methyl alcohol methyl oxirane methyl acetate butyraldehyde |
11 12 13 14 15 16 17 | Enanthaldehyde 2-valeral---octanal- |
8 9 10 | Hexanal furfural 2,6- |
18 | 3-Ethyl-2-Methyl-1,3-hexadiene |
The methodological study of experimental example 2, Bupleurum injection
Precision test
Choose sample continuous sample introduction 5 pins of same lot number, measure finger-print, adopt its similarity of finger-print software evaluation.Its finger-print and similarity are shown in respectively Fig. 3 and table 3.As can be seen from Table 3, similarity is 1, illustrates that sampling instrument precision is good.
Table 3 radix bupleuri finger-print precision is investigated similarity result of calculation
1 | 2 | 3 | 4 | 5 | Reference fingerprint | |
1 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
2 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
3 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
4 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
5 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
Reference fingerprint | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
2, stability test
Choose same sample solution respectively at 0,1,2,4,8 hour sample introduction, measure finger-print, adopt its similarity of finger-print software evaluation.Its finger-print and similarity are shown in respectively Fig. 4 and table 4.As can be seen from Table 4, similarity is 1, and interpret sample solution is stable in 8 hours.
Table 4 radix bupleuri finger-print study on the stability similarity result of calculation
0 hour | 1 hour | 2 hours | 4 hours | 8 hours | Reference fingerprint | |
0 hour | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
1 hour | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
2 hours | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
4 hours | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
8 hours | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
Reference fingerprint | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
3, replica test
Get same lot number repetitive operation 5 times, its repeatability investigates collection of illustrative plates and similarity result of calculation is shown in respectively Fig. 5 and table 5.As can be seen from Table 5, its similarity is 1, illustrates that the method repeatability is fine.
Table 5 radix bupleuri reproducibility of fingerprint is investigated similarity result of calculation
1 | 2 | 3 | 4 | 5 | Reference fingerprint | |
1 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
2 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
3 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
4 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
5 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
Reference fingerprint | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
4, the detection of sample:
According to the inventive method, utilize the finger-print set up to analyze the Bupleurum injection of commercially available 30Ge producer, the results are shown in Table 6.
The similarity result of calculation of each enterprise's Bupleurum injection finger-print of table 6 and reference fingerprint
Enterprise | Similarity | Enterprise | Similarity | Enterprise | Similarity |
123456789 10 mean values | 0.990 0.947 0.935 0.785 0.973 0.737 0.905 0.945 0.904 0.931 0.879 | 11 12 13 14 15 16 17 18 19 20 | 0.637 0.980 0.956 0.960 0.907 0.930 0.661 0.947 0.840 0.913 | 21 22 23 24 25 26 27 28 29 30 | 0.747 0.968 0.983 0.942 0.915 0.952 0.559 0.921 0.837 0.778 |
As can be seen from the above table, the fingerprint similarity value of each enterprise's sample is between 0.54-0.99, and the production technology of declaratives enterprise still exists certain problem, requires further improvement, improves; The comprehensive testing result of sample of enterprise's production and the changeability of the volatile ingredient of Radix Bupleuri analyzed, the similarity value of suggestion Bupleurum injection finger-print is fixed tentatively as being not less than 0.7.
Claims (5)
1. the detection method of Bupleurum injection, comprises the steps:
The first step, vapor-phase chromatography is set up Bupleurum injection reference fingerprint: adopt nonpolar or low pole quartz capillary column, with N
2for carrier gas, flow velocity 0.8-1.5mL/min, current constant mode, split ratio is 10-20:1; Take FID as detecting device, adopt the mode of temperature programme to analyze; Need testing solution injecting chromatograph by least 10 batches of Bupleurum injections, records chromatogram, utilizes fingerprint similarity evaluation software to generate Bupleurum injection reference fingerprint;
Second step, measures by the first step method finger-print that Bupleurum injection detects sample;
The 3rd step, calculates Bupleurum injection and detects the finger-print of sample and the similarity of reference fingerprint;
Described need testing solution is prepared by the process of following A or B:
A, precision are drawn 10ml Bupleurum injection with heavily steaming ether equivalent extracting twice, each 10ml, and combined ether layer, adds anhydrous sodium sulfate dehydration 30 minutes, filters, and filtrate vacuum is drained, and residue is 5ml with heavily steaming ether dissolution constant volume, obtains described need testing solution;
B, the accurate Bupleurum injection 1.0ml that draws, put in 10ml head space bottle, seals, and obtains need testing solution;
Wherein, adopt the condition of headspace sampling mode to be: head space bottle temperature 80-90 ℃, sampling valve temperature 90-120 ℃, transmission line temperature 110-120 ℃; Head space bottle equilibration time 10-25min, head space bottle pressurising time 0.1-0.5min, quantitatively ring filling time 0.1-0.5min, quantitatively encircles equilibration time 0.2-1.0min, sample injection time 0.5-2.0min;
The mode of chromatographic column adopting temperature programme is analyzed, and the condition of temperature programme is: initial 35 ℃, keep 2min; 1 ℃/min rises to 40 ℃, keeps 2min, and 3 ℃/min rises to 60 ℃, keeps 3min, and 7 ℃/min rises to 200 ℃, keeps 3min.
2. detection method according to claim 1, is characterized in that: being take in No. 6 valeral peaks at the total peak in described Bupleurum injection reference fingerprint is reference, and relative retention time and the relative peak area at each total peak are as follows:
No. 1 peak relative retention time is 0.500 ± 0.001, relative peak area 45.673 ± 100.619; No. 2 peak relative retention time is 0.527 ± 0.001, and relative peak area is 98.828 ± 343.681; No. 3 peak relative retention time is 0.553 ± 0.002, and relative peak area is 1.308 ± 1.898; No. 4 peak relative retention time is 0.677 ± 0.002, and relative peak area is 0.320 ± 0.229; No. 5 peak relative retention time is 0.838 ± 0.004, and relative peak area is 0.285 ± 0.293; No. 6 peak is 1.000 ± 0.000, and relative peak area is 1.000 ± 0.000; No. 7 peak relative retention time is 1.467 ± 0.006, and relative peak area is 0.386 ± 0.406; No. 8 peak relative retention time is 1.724 ± 0.002, and relative peak area is 1.947 ± 1.498; No. 9 peak relative retention time is 2.040 ± 0.006, and relative peak area is 0.837 ± 1.964; No. 10 peak relative retention time is 2.414 ± 0.008, and relative peak area is 0.697 ± 0.750; No. 11 peak relative retention time is 2.716 ± 0.006, and relative peak area is 0.639 ± 0.431; No. 12 peak relative retention time is 3.335 ± 0.010, and relative peak area is 0.300 ± 0.477; No. 13 peak relative retention time is 3.465 ± 0.011, and relative peak area is 0.241 ± 0.245; No. 14 peak relative retention time is 3.531 ± 0.013, and relative peak area is 0.182 ± 0.357; No. 15 peak relative retention time is 3.695 ± 0.013, and relative peak area is 0.161 ± 0.175; No. 16 peak relative retention time is 3.941 ± 0.018, and relative peak area is 0.149 ± 0.201; No. 17 peak relative retention time is 4.030 ± 0.015, and relative peak area is 0; 240 ± 0.299; No. 18 peak relative retention time is 4.105 ± 0.016, and relative peak area is 0.208 ± 0.221.
3. detection method according to claim 1, is characterized in that: while setting up Bupleurum injection reference fingerprint, generally choose the Radix Bupleuri in the genuine place of production and make Bupleurum injection according to following step:
Get the genuine Radix Bupleuri 1000g that is no more than half a year storage period, be cut into a cun section, rinse well, add the purified water of 11 times of amounts, 70 ℃ of temperature are soaked 8 hours; Through steam distillation, collect just distillate of 6000mL, then re-distillation, collect double distilled liquid, about 1000mL; Add 3.0g Tween-80, stir oil is dissolved completely, then add 9.0g sodium chloride, after dissolving, filter, inject water to 1000mL, with 10% sodium hydroxide solution, regulate pH value to 7.0, with 0.45 μ m miillpore filter, filter, embedding, 100 ℃ of sterilizings 30 minutes, obtain Bupleurum injection.
4. detection method according to claim 1, is characterized in that: described quartz capillary column is that dimethyl siloxane is the fixing quartz capillary column of phase.
5. detection method according to claim 1, is characterized in that: FID testing conditions is: injector temperature is 220-250 ℃, and detector temperature is 250-270 ℃.
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CN1588049A (en) * | 2004-09-27 | 2005-03-02 | 上海中药创新研究中心 | Method for producing Chinese medicine fingerprint atlas |
CN1899333A (en) * | 2005-07-25 | 2007-01-24 | 郭爱华 | Bupleurum root extract, its preparing method and its use |
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Patent Citations (2)
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CN1588049A (en) * | 2004-09-27 | 2005-03-02 | 上海中药创新研究中心 | Method for producing Chinese medicine fingerprint atlas |
CN1899333A (en) * | 2005-07-25 | 2007-01-24 | 郭爱华 | Bupleurum root extract, its preparing method and its use |
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王欣月.柴荆注射液中药材的指纹图谱研究及含量测定.《中国优秀硕士学位论文全文数据库》.2006,15-46. |
生药挥发油的气相色谱鉴定;杨维稼;《中日友好医院学报》;19880930;第2卷(第3期);135-139 * |
肖蓉 等.不同产地柴胡药材GC-MS指纹图谱研究.《中草药》.2006,第37卷(第8期),1248-1252. |
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