CN101013110A - 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 Bupleurum injection quality control method, particularly relate to employing fingerprint collection of illustrative plates control Bupleurum injection method for 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 heatings such as flu, influenza and malaria in a large number, has definite curative effect.At present, mainly be to check absorbance log and pH value for Bupleurum injection quality control method, absorbance log: precision is measured parenteral solution 5ml, puts in the 50ml measuring bottle, and thin up shakes up to scale, as need testing solution.Precision is measured parenteral solution 5ml in addition, puts in the evaporating dish, and evaporate to dryness in water-bath adds water and makes dissolving, moves in the 50ml measuring bottle, and thin up shakes up to scale, as blank.Measure according to spectrophotometric method (" Drug Standard of Ministry of Public Health of the Peoples Republic of China " appendix V A), at 278nm and 243nm wavelength place absorption maximum and minimal absorption are arranged respectively, 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 we studies show that, the detection of this detection method medium ultraviolet absorbance log is actually the reflection of toxic ingredient furfural, and this detection method does not have specificity discriminating and assay etc. than the effective quality control method; What parenteral solution was used in addition is the aqua aromatica of radix bupleuri medicinal material through the distillation gained, mainly contains volatile ingredient, and its quality is unstable more, has had a strong impact on the clinical efficacy and the security of this medicine.
Summary of the invention
The purpose of this invention is to provide a kind of Bupleurum injection quality control method, particularly utilize the finger-print of Bupleurum injection to carry out Bupleurum injection quality control method.
Bupleurum injection quality control method of the present invention comprises the steps:
The first step, vapor-phase chromatography are set up the Bupleurum injection reference fingerprint: adopt nonpolar or low pole quartz capillary column, with N
2Be carrier gas, flow velocity 0.8-1.5mL/min, current constant mode, split ratio is 10-20: 1; With FID is detecting device, adopts the mode of temperature programme to analyze; With the need testing solution injecting chromatograph of at least 10 batches of Bupleurum injections, the record chromatogram utilizes finger-print similarity evaluation software to generate the Bupleurum injection reference fingerprint;
Second step is by the finger-print of first step method mensuration Bupleurum injection test sample;
The 3rd step, calculate the finger-print of Bupleurum injection test sample and the similarity of reference fingerprint, similarity is greater than the specification product that are more than 0.7.
In above-mentioned steps 1) when setting up the Bupleurum injection reference fingerprint, generally choose the radix bupleuri medicinal material in the genuine place of production and make Bupleurum injection according to following step:
Promptly get the genuine radix bupleuri medicinal material 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 were soaked 8 hours.Through steam distillation, collect 6000mL distillate just, distillation is again collected double distilled liquid, about 1000mL again.Add the 3.0g Tween-80, stirring is dissolved oil fully, adds 9.0g sodium chloride again, after the dissolving, filter, add the injection water, regulate pH value to 7.0, filter with 0.45 μ m miillpore filter with 10% sodium hydroxide solution to 1000mL, embedding was sterilized 30 minutes, and was promptly got Bupleurum injection for 100 ℃.Preparation method according to the Bupleurum injection need testing solution prepares need testing solution then.
Wherein, the finger-print of gained of the present invention as shown in Figure 2, each total peak is reference with the valeral peak, ((the relative peak area ± SD) as follows of keeping: No. 1 the peak relative retention time is 0.500 ± 0.001, relative peak area 45.673 ± 100.619 for relative retention time ± SD) and relative peak area to calculate relative retention time; No. 2 the peak relative retention time is 0.527 ± 0.001, and relative peak area is 98.828 ± 343.681; No. 3 the peak relative retention time is 0.553 ± 0.002, and relative peak area is 1.308 ± 1.898; No. 4 the peak relative retention time is 0.677 ± 0.002, and relative peak area is 0.320 ± 0.229; No. 5 the peak relative retention time is 0.838 ± 0.004, and relative peak area is 0.285 ± 0.293; No. 6 the peak is 1.000 ± 0.000, and relative peak area is 1.000 ± 0.000; No. 7 the peak relative retention time is 1.467 ± 0.006, and relative peak area is 0.386 ± 0.406; No. 8 the peak relative retention time is 1.724 ± 0.002, and relative peak area is 1.947 ± 1.498; No. 9 the peak relative retention time is 2.040 ± 0.006, and relative peak area is 0.837 ± 1.964; No. 10 the peak relative retention time is 2.414 ± 0.008, and relative peak area is 0.697 ± 0.750; No. 11 the peak relative retention time is 2.716 ± 0.006, and relative peak area is 0.639 ± 0.431; No. 12 the peak relative retention time is 3.335 ± 0.010, and relative peak area is 0.300 ± 0.477; No. 13 the peak relative retention time is 3.465 ± 0.011, and relative peak area is 0.241 ± 0.245; No. 14 the peak relative retention time is 3.531 ± 0.013, and relative peak area is 0.182 ± 0.357; No. 15 the peak relative retention time is 3.695 ± 0.013, and relative peak area is 0.161 ± 0.175; No. 16 the peak relative retention time is 3.941 ± 0.018, and relative peak area is 0.149 ± 0.201; No. 17 the peak relative retention time is 4.030 ± 0.015, and relative peak area is 0.240 ± 0.299; No. 18 the 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 the quartz capillary column that dimethyl siloxane is a stationary phase.
The 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 the 10ml head space bottle, and seal, promptly get need testing solution.Wherein, adopt the condition of headspace sampling mode to be: 80-90 ℃ of head space bottle temperature, 90-120 ℃ of sampling valve temperature, 110-120 ℃ of transmission line temperature; 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 need testing solution preparation method is except that headspace sampling, can also adopt direct injected behind the organic solvent extraction, concrete operations are: the accurate 10ml Bupleurum injection of drawing, with heavily steaming ether equivalent extracting twice, each 10ml, combined ether layer, added anhydrous sodium sulfate dehydration 30 minutes, and filtered, the filtrate vacuum is drained, residue is 5ml with heavily steaming ether dissolution and constant volume, obtains described need testing solution.
The present invention is by setting up the finger-print of Bupleurum injection, the employing fingerprint collection of illustrative plates is controlled the quality of Bupleurum injection, have good reproducibility, stable advantages of higher, but the quality of effective monitoring Bupleurum injection, can guarantee the stable, consistent of Bupleurum injection clinical efficacy, have important use and be worth.
Description of drawings
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 contains volatile ingredient, and it is proper therefore to adopt the GC-FID method to set up finger-print.
2, the investigation of chromatographic column:
Respectively to Agilent HP-530m * 0.32mm * 0.25 μ m (low pole); Agilent DB-WAX 30m * 0.53mm * 1 μ m (strong polarity); Agilent DB-624 30m * 0.32mm * three kinds of gas phase capillary columns of 1.8 μ m (nonpolar) are investigated, the 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, wherein best with HP-5 capillary column (dimethyl siloxane is a stationary phase) separating effect again.
3, the preparation method of need testing solution:
We have investigated hand sampling behind headspace sampling and the organic solvent extraction, find that dual mode all can realize the detection of finger-print.
The 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 added anhydrous sodium sulfate dehydration 30 minutes, filtered, the filtrate vacuum is drained, and residue is that 5ml is standby with heavily steaming ether dissolution and 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 the 10ml head space bottle, seal, promptly.
The condition of headspace sampling is: 80-90 ℃ of head space bottle temperature, 90-120 ℃ of sampling valve temperature, 110-120 ℃ of transmission line temperature; 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
With hand sampling or through the head-space sampler sample introduction, inject gas chromatograph writes down 42 minutes chromatogram with the Bupleurum injection test sample.
With N2 is carrier gas, flow velocity 0.8-1.5mL/min, and current constant mode, split ratio is 10: 1-20: 1; With FID is 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 medicinal material 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 were soaked 8 hours.Through steam distillation, collect 6000mL distillate just, distillation is again collected double distilled liquid, about 1000mL again.Add the 3.0g Tween-80, stirring is dissolved oil fully, adds 9.0g sodium chloride again, after the dissolving, filter, add the injection water, regulate pH value to 7.0, filter with 0.45 μ m miillpore filter with 10% sodium hydroxide solution to 1000mL, embedding was sterilized 30 minutes, and was promptly got Bupleurum injection for 100 ℃.
Prepare 10 batches parenteral solution by the preparation method of Bupleurum injection, measure its finger-print, the 10 crowdes of Bupleurum injection sample finger-print stacking diagrams such as Fig. 1.Adopt similarity evaluation software that 10 batches of Bupleurum injection sample finger-prints are carried out similarity and calculate, the results are shown in Table 1.
Utilize similarity software to generate the common pattern of Bupleurum injection sample finger-print, promptly get reference fingerprint, as Fig. 2.Utilize GC-MS that the chromatographic peak in the Bupleurum injection is pointed out, each peak ownership sees Table 2.
Among Fig. 2, each total peak is reference with No. 6 peak-valeral peaks, calculate relative retention time (relative retention time ± SD) and relative peak area (the relative peak area ± SD) of keeping:
No. 1 the peak relative retention time is 0.500 ± 0.001, relative peak area 45.673 ± 100.619; No. 2 the peak relative retention time is 0.527 ± 0.001, and relative peak area is 98.828 ± 343.681; No. 3 the peak relative retention time is 0.553 ± 0.002, and relative peak area is 1.308 ± 1.898; No. 4 the peak relative retention time is 0.677 ± 0.002, and relative peak area is 0.320 ± 0.229; No. 5 the peak relative retention time is 0.838 ± 0.004, and relative peak area is 0.285 ± 0.293; No. 6 the peak is 1.000 ± 0.000, and relative peak area is 1.000 ± 0.000; No. 7 the peak relative retention time is 1.467 ± 0.006, and relative peak area is 0.386 ± 0.406; No. 8 the peak relative retention time is 1.724 ± 0.002, and relative peak area is 1.947 ± 1.498; No. 9 the peak relative retention time is 2.040 ± 0.006, and relative peak area is 0.837 ± 1.964; No. 10 the peak relative retention time is 2.414 ± 0.008, and relative peak area is 0.697 ± 0.750; No. 11 the peak relative retention time is 2.716 ± 0.006, and relative peak area is 0.639 ± 0.431; No. 12 the peak relative retention time is 3.335 ± 0.010, and relative peak area is 0.300 ± 0.477; No. 13 the peak relative retention time is 3.465 ± 0.011, and relative peak area is 0.241 ± 0.245; No. 14 the peak relative retention time is 3.531 ± 0.013, and relative peak area is 0.182 ± 0.357; No. 15 the peak relative retention time is 3.695 ± 0.013, and relative peak area is 0.161 ± 0.175; No. 16 the peak relative retention time is 3.941 ± 0.018, and relative peak area is 0.149 ± 0.201; No. 17 the peak relative retention time is 4.030 ± 0.015, and relative peak area is 0.240 ± 0.299; No. 18 the peak relative retention time is 4.105 ± 0.016, and relative peak area is 0.208 ± 0.221.
10 batches of Bupleurum injection samples of table 1 finger-print similarity result of calculation table
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 the ownership table
Peak number | The composition title | Peak number | The composition title |
1 | |
11 | Enanthaldehyde |
2 | |
12 | The 2-valeral |
3 | Methyl oxirane | 13 | - |
4 | Methyl acetate | 14 | - |
5 | Butyraldehyde | 15 | - |
6 | Valeral | 16 | Octanal |
7 | Amylalcohol | 17 | - |
8 | Hexanal | 18 | 3-ethyl-2-methyl isophthalic acid, the 3-hexadiene |
9 | Furfural | ||
10 | 2,6-dimethyl heptene |
The methodological study of experimental example 2, Bupleurum injection
The 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 seen Fig. 3 and table 3 respectively.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 seen Fig. 4 and table 4 respectively.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 | 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 seen Fig. 5 and table 5 respectively.As can be seen from Table 5, its similarity is 1, illustrates that this method repeatability is fine.
Table 5 radix bupleuri finger-print reappearance 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 of being set up that the Bupleurum injection of commercially available 30 producers is analyzed, 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 |
1 | 0.990 | 11 | 0.637 | 21 | 0.747 |
2 | 0.947 | 12 | 0.980 | 22 | 0.968 |
3 | 0.935 | 13 | 0.956 | 23 | 0.983 |
4 | 0.785 | 14 | 0.960 | 24 | 0.942 |
5 | 0.973 | 15 | 0.907 | 25 | 0.915 |
6 | 0.737 | 16 | 0.930 | 26 | 0.952 |
7 | 0.905 | 17 | 0.661 | 27 | 0.559 |
8 | 0.945 | 18 | 0.947 | 28 | 0.921 |
9 | 0.904 | 19 | 0.840 | 29 | 0.837 |
10 | 0.931 | 20 | 0.913 | 30 | 0.778 |
Mean value | 0.879 |
As can be seen from the above table, the finger-print 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 changeability of the test result of samples that analysis-by-synthesis enterprise produces and the volatile ingredient of radix bupleuri medicinal material, the similarity value of suggestion Bupleurum injection finger-print is tentative for should be not less than 0.7.
Claims (9)
1, Bupleurum injection quality control method comprises the steps:
The first step, vapor-phase chromatography are set up the Bupleurum injection reference fingerprint: adopt nonpolar or low pole quartz capillary column, with N
2Be carrier gas, flow velocity 0.8-1.5mL/min, current constant mode, split ratio is 10-20: 1; With FID is detecting device, adopts the mode of temperature programme to analyze; With the need testing solution injecting chromatograph of at least 10 batches of Bupleurum injections, the record chromatogram utilizes finger-print similarity evaluation software to generate the Bupleurum injection reference fingerprint;
Second step is by the finger-print of first step method mensuration Bupleurum injection test sample;
The 3rd step, calculate the finger-print of Bupleurum injection test sample and the similarity of reference fingerprint, similarity is greater than the specification product that are more than 0.7.
2, method of quality control according to claim 1 is characterized in that: the total peak in the described Bupleurum injection reference fingerprint is reference with No. 6 valeral peaks, and the relative retention time and the relative peak area at each total peak are as follows:
No. 1 the peak relative retention time is 0.500 ± 0.001, relative peak area 45.673 ± 100.619; No. 2 the peak relative retention time is 0.527 ± 0.001, and relative peak area is 98.828 ± 343.681; No. 3 the peak relative retention time is 0.553 ± 0.002, and relative peak area is 1.308 ± 1.898; No. 4 the peak relative retention time is 0.677 ± 0.002, and relative peak area is 0.320 ± 0.229; No. 5 the peak relative retention time is 0.838 ± 0.004, and relative peak area is 0.285 ± 0.293; No. 6 the peak is 1.000 ± 0.000, and relative peak area is 1.000 ± 0.000; No. 7 the peak relative retention time is 1.467 ± 0.006, and relative peak area is 0.386 ± 0.406; No. 8 the peak relative retention time is 1.724 ± 0.002, and relative peak area is 1.947 ± 1.498; No. 9 the peak relative retention time is 2.040 ± 0.006, and relative peak area is 0.837 ± 1.964; No. 10 the peak relative retention time is 2.414 ± 0.008, and relative peak area is 0.697 ± 0.750; No. 11 the peak relative retention time is 2.716 ± 0.006, and relative peak area is 0.639 ± 0.431; No. 12 the peak relative retention time is 3.335 ± 0.010, and relative peak area is 0.300 ± 0.477; No. 13 the peak relative retention time is 3.465 ± 0.011, and relative peak area is 0.241 ± 0.245; No. 14 the peak relative retention time is 3.531 ± 0.013, and relative peak area is 0.182 ± 0.357; No. 15 the peak relative retention time is 3.695 ± 0.013, and relative peak area is 0.161 ± 0.175; No. 16 the peak relative retention time is 3.941 ± 0.018, and relative peak area is 0.149 ± 0.201; No. 17 the peak relative retention time is 4.030 ± 0.015, and relative peak area is 0.240 ± 0.299; No. 18 the peak relative retention time is 4.105 ± 0.016, and relative peak area is 0.208 ± 0.221.
3, method of quality control according to claim 1 is characterized in that: when setting up the Bupleurum injection reference fingerprint, generally choose the radix bupleuri medicinal material in the genuine place of production and make Bupleurum injection according to following step:
Get the genuine radix bupleuri medicinal material 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 were soaked 8 hours; Through steam distillation, collect 6000mL distillate just, distillation is again collected double distilled liquid, about 1000mL again; Add the 3.0g Tween-80, stirring is dissolved oil fully, adds 9.0g sodium chloride again, after the dissolving, filter, add the injection water, regulate pH value to 7.0, filter with 0.45 μ m miillpore filter with 10% sodium hydroxide solution to 1000mL, embedding was sterilized 30 minutes, and was promptly got Bupleurum injection for 100 ℃.
4, method of quality control according to claim 1 is characterized in that: described quartz capillary column is that dimethyl siloxane is the quartz capillary column of stationary phase.
5, method of quality control according to claim 1 is characterized in that: the FID testing conditions is: injector temperature is 220-250 ℃, and detector temperature is 250-270 ℃.
6, method of quality control according to claim 1 is characterized in that: 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.
7, method of quality control according to claim 1 is characterized in that: described need testing solution prepares according to the following procedure:
The accurate 10ml Bupleurum injection of drawing is with heavily steaming ether equivalent extracting twice, each 10ml, and combined ether layer added anhydrous sodium sulfate dehydration 30 minutes, filtration, the filtrate vacuum is drained, and residue is 5ml with heavily steaming ether dissolution and constant volume, obtains described need testing solution.
8, method of quality control according to claim 1 is characterized in that: described need testing solution prepares according to the following procedure:
The accurate Bupleurum injection 1.0ml that draws puts in the 10ml head space bottle, seals, and promptly gets need testing solution.
9, method of quality control according to claim 8 is characterized in that: the sample injecting chromatograph, adopt the headspace sampling mode, and the condition of headspace sampling is: 80-90 ℃ of head space bottle temperature, 90-120 ℃ of sampling valve temperature, 110-120 ℃ of transmission line temperature; 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.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103197003A (en) * | 2012-01-04 | 2013-07-10 | 天士力制药集团股份有限公司 | Authentication method of Chinese thorowax root medicine material |
CN107727785A (en) * | 2017-11-10 | 2018-02-23 | 吉林修正药业新药开发有限公司 | A kind of construction method of Chinese patent drug Toxin-Vanquishing particle gas phase characteristic collection of illustrative plates |
CN110702808A (en) * | 2019-09-25 | 2020-01-17 | 中国兽医药品监察所 | Quality inspection method of radix bupleuri and asarum in chaihin injection |
CN111089913A (en) * | 2019-10-16 | 2020-05-01 | 四川恒通动保生物科技有限公司 | Quality control method of bupleurum chinense injection |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
-
2007
- 2007-01-25 CN CN200710063047.2A patent/CN101013110B/en not_active Expired - Fee Related
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
Non-Patent Citations (5)
Title |
---|
李秀琴 等: "柴胡挥发油质量的GC指纹图谱分析方法", 《中草药》 * |
李秀琴: "柴胡质量评价方法与其相关成分的药动学研究", 《中国博士论文全文数据库》 * |
杨维稼: "生药挥发油的气相色谱鉴定", 《中日友好医院学报》 * |
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》 * |
肖蓉 等: "不同产地柴胡药材GC-MS指纹图谱研究", 《中草药》 * |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103197003A (en) * | 2012-01-04 | 2013-07-10 | 天士力制药集团股份有限公司 | Authentication method of Chinese thorowax root medicine material |
CN103197003B (en) * | 2012-01-04 | 2016-03-02 | 天士力制药集团股份有限公司 | A kind of authentication method of Radix Bupleuri |
CN107727785A (en) * | 2017-11-10 | 2018-02-23 | 吉林修正药业新药开发有限公司 | A kind of construction method of Chinese patent drug Toxin-Vanquishing particle gas phase characteristic collection of illustrative plates |
CN110702808A (en) * | 2019-09-25 | 2020-01-17 | 中国兽医药品监察所 | Quality inspection method of radix bupleuri and asarum in chaihin injection |
CN111089913A (en) * | 2019-10-16 | 2020-05-01 | 四川恒通动保生物科技有限公司 | Quality control method of bupleurum chinense injection |
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