CN102023188A - Quality control method of scutellarin - Google Patents
Quality control method of scutellarin Download PDFInfo
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- CN102023188A CN102023188A CN 200910176215 CN200910176215A CN102023188A CN 102023188 A CN102023188 A CN 102023188A CN 200910176215 CN200910176215 CN 200910176215 CN 200910176215 A CN200910176215 A CN 200910176215A CN 102023188 A CN102023188 A CN 102023188A
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Abstract
The invention provides a quality control method of scutellarin. The method comprises the following steps of: providing a test sample solution for measuring the scutellarin content; detecting the test sample solution in a liquid-phase chromatographic instrument by using octadecyl silane bonded silica or octadecylsilane bonded silica as a filler and using the mixed solution of methanol, tetrahydrofuran and a phosphoric acid solution as a moving phase; and obtaining the scutellarin content through analysis by using an external reference method. By using the quality control method, the scutellarin mass in the scutellarin preparation process can be accurately estimated so as to finally obtain the scutellarin with stable quality.
Description
Technical field
The present invention is relevant with the preparation technology of lamp-dish flower acetic, is specifically related to a kind of method of quality control of lamp-dish flower acetic.
Background technology
Fleabane flower has another name called erigeron breviscapus, gains the name like the root of Chinese wild ginger like oil lamp, root because of flower, is the herb of the short booth bitter fleabane of composite family bitter fleabane platymiscium [Erigeron breviscapus (vant.) Hand-Mazz].This medicinal material head is stated from " the southern regions of the Yunnan Province book on Chinese herbal medicine ", has recorded in that " Chinese pharmacopoeia version in 2005, Yunnan is among the people to be usually used in treating traumatic injury, rheumatalgia pain, toothache, stomachache, flu etc.Nineteen seventies, through clinical verification, fleabane flower has better curative effect to hypertension, cerebral hemorrhage, cerebral thrombosis, cerebral embolism polyneuropathy, chronic archnoiditis and sequelae thereof, and rheumatism, coronary heart disease are also had certain curative effect.
The research of fleabane flower has been determined that the main active of treatment cardiovascular and cerebrovascular disease in the fleabane flower is Breviscapinun (Breviscapine), Breviscapinun mainly contains oil lamp cycle of sixty years element (Apigenin-7-O-glucuronside, structural formula I) and lamp-dish flower acetic (Scutellarin, have another name called scutellarin, molecular formula C
21H
18O
12, molecular weight is 462.37, structural formula II).Result of study confirms that further the lamp-dish flower acetic treatment cardiovascular and cerebrovascular disease drug effect in the Breviscapinun is definite.
For traditional Chinese medicine, big and composition is unclear owing to medicinal material batch differences etc., and reason causes occurring bad reaction easily.At present, the commercially available injection of being made by fleabane flower has produced a lot of bad reactions (being called for short ADR), bad reaction about the fleabane flower injection is also put on record at national bad reaction center, and commercially available fleabane flower injection mainly is divided into Breviscapini injection (powder pin), fleabane injection, fleabane injection, erigeron breviscapus parenteral solution.
Fleabane flower injection ADR reports demonstration, and system damage comprises due to the fleabane flower injection: the infringement of maincenter and peripheral neverous system, gastronintestinal system, systemic circulation system, liver and gall, respiratory system, skin and annex etc.It is high with effective constituent and purity is not high relevant that a major reason of above-mentioned bad reaction takes place the fleabane flower injection.
The bad reaction situation of the injection of making in view of being used as medicine with Breviscapinun, and result of study confirmed that the main effective constituent of fleabane flower injection is lamp-dish flower acetic, therefore is necessary to prepare the fleabane flower injection that main effective constituent is lamp-dish flower acetic.Further, in the process of preparation lamp-dish flower acetic, need control the quality of lamp-dish flower acetic, thereby the lamp-dish flower acetic quality is estimated accurately, be beneficial to the stable lamp-dish flower acetic of preparation quality, be the clinical and non-clinical study reduction risk of lamp-dish flower acetic, and finally reduce the bad reaction of medicine.
Summary of the invention
The technical matters that the present invention solves is, a kind of method of quality control of lamp-dish flower acetic is provided, and by this method of quality control, the quality of described lamp-dish flower acetic is estimated accurately, to help the stable lamp-dish flower acetic of preparation quality.
In order to solve above technical matters, the invention provides a kind of method of quality control of lamp-dish flower acetic, comprising:
The assay need testing solution of lamp-dish flower acetic is provided;
With octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels is filling agent, with the mixed liquor of methyl alcohol, tetrahydrofuran and phosphate aqueous solution as moving phase, detect described need testing solution in liquid chromatograph, the external standard method analysis obtains the content of described lamp-dish flower acetic.
Preferably, the concentration of described phosphate aqueous solution is 0.05wt%～0.25wt%.
Preferably, be methyl alcohol in the mixed solution of described methyl alcohol, tetrahydrofuran and phosphate aqueous solution by volume: tetrahydrofuran: phosphate aqueous solution is 21～25: 8～12: 65～70.
Preferably, the described number of theoretical plate that detects described need testing solution in chromatograph calculates by the lamp-dish flower acetic peak and is not less than 5000.
Preferably, the described detection wavelength that the described need testing solution of detection uses in chromatograph is 330nm～340nm.
Preferably, described method of quality control also comprises the step that detects its related substances in the described lamp-dish flower acetic, and the step of related substance specifically comprises in the described lamp-dish flower acetic of described detection:
Lamp-dish flower acetic related substance inspection need testing solution is provided;
Get described need testing solution dilution and obtain contrast solution;
Get described contrast solution and need testing solution and in liquid chromatography, analyze, contrast the related substance peak area of described test sample liquid and the main peak area of described contrast solution, obtain the content of described related substance.
Preferably, describedly get described contrast solution and related substance inspection and detect the stationary phase that uses with need testing solution be octadecylsilane bonding or eight alkyl silane bonded silica gels in liquid chromatography, moving phase is the mixed liquor of methyl alcohol, tetrahydrofuran and phosphate aqueous solution.
Preferably, the described time when getting described contrast solution and need testing solution and analyzing in liquid chromatography is more than 2 times of lamp-dish flower acetic major component peak retention time.
Preferably, in the step of its related substances, the concentration of described need testing solution is 0.1mg/ml～0.3mg/ml in the described lamp-dish flower acetic of described detection.
Preferably, in the step of its related substances, the concentration of described contrast solution is 2 μ g/ml～10 μ g/ml in the described lamp-dish flower acetic of described detection.
Preferably, in the described lamp-dish flower acetic of described detection in the step of its related substances, described described contrast solution and the need testing solution got analyzed in liquid chromatography and specifically comprised:
Get described reference substance solution and inject liquid chromatograph, make the major component peak height be about 10% of registering instrument full scale;
Get described contrast solution and described need testing solution 5-20 μ l injecting chromatograph, the related substance peak of described need testing solution is all shown.
Preferably, described method of quality control also comprise with described lamp-dish flower acetic Cu-K α target emanation,
Carry out X-ray diffraction under the condition of 2 θ=2 °～70 ° and detect, confirm whether to possess X ray diffracting spectrum as described in Table 1:
The X ray diffracting spectrum of table 1, lamp-dish flower acetic
Preferably, described method of quality control also comprises described lamp-dish flower acetic is carried out infrared detection, confirms whether to have following wave number (cm
-1): 3511 ± 2,3373 ± 2,2920 ± 2,2885 ± 2,1721 ± 2,1662 ± 2,1608 ± 2,1575 ± 2,1498 ± 2,1467 ± 2,1442 ± 2,1400 ± 2,1362 ± 2,1286 ± 2,1249 ± 2,1224 ± 2,1183 ± 2,1150 ± 2,1119 ± 2,1101 ± 2,1084 ± 2,1041 ± 2,846 ± 2,813 ± 2,740 ± 2,720 ± 2,618 ± 2.
Preferably, whether described method of quality control also comprises the step of described Breviscapinun being carried out the test of DSC endothermic transition, be 124 ℃～128 ℃ to confirm described lamp-dish flower acetic endothermic transition temperature.
Preferably, whether described method of quality control also comprises described lamp-dish flower acetic is carried out thermogravimetric-differential thermal analysis (DTA), be 207 ℃～209 ℃ to confirm its fusion and decomposition temperature, and whether confirms the mass attenuation with 12%～15%.
The invention provides a kind of method of quality control of lamp-dish flower acetic.In described method of quality control, with octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels is filling agent, mixed liquor with methyl alcohol, tetrahydrofuran and phosphate aqueous solution is a moving phase, detect described need testing solution in liquid chromatograph, external standard method obtains the content of described lamp-dish flower acetic.By described method of quality control, can in preparation lamp-dish flower acetic process, the quality of lamp-dish flower acetic be estimated accurately, to guarantee finally to obtain stay-in-grade lamp-dish flower acetic.
Description of drawings
Fig. 1 is the chromatogram of the lamp-dish flower acetic content of measurement in the embodiment of the invention 1;
Fig. 2 is the lamp-dish flower acetic related substance inspection test sample chromatogram of measuring in the embodiment of the invention 2;
Fig. 3 is the lamp-dish flower acetic related substance inspection contrast solution chromatogram of measuring in the embodiment of the invention 2;
Fig. 4 is the X-ray diffractogram of the lamp-dish flower acetic of the embodiment of the invention 3 tests;
Fig. 5 is the infrared spectrum of the lamp-dish flower acetic of the embodiment of the invention 4 tests;
Fig. 6 is the DSC-TGA curve map of the lamp-dish flower acetic of the embodiment of the invention 5 tests.
Embodiment
The embodiment of the method for quality control of a lamp-dish flower acetic provided by the invention comprises:
Lamp-dish flower acetic assay need testing solution is provided;
Be filling agent, be moving phase with octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels with the mixed liquor of methyl alcohol, tetrahydrofuran and phosphate aqueous solution, detect the described trial target solution that supplies in liquid chromatograph, the external standard method analysis obtains the content of described lamp-dish flower acetic.
Breviscapinun of the present invention is any one in plant separation and purification or the chemosynthesis.According to the present invention, described lamp-dish flower acetic assay is meant with need testing solution lamp-dish flower acetic is dissolved in the solution that organic solvent obtains, and described organic solvent can be lower alcohol, and described lower alcohol can be methyl alcohol, ethanol, propyl alcohol.For the concentration of described need testing solution, be preferably 40 μ g/ml～60 μ g/ml, more preferably 45 μ g/ml～55 μ g/ml, more preferably 48 μ g/ml～52 μ g/ml.
According to the present invention, in liquid chromatography, detect described need testing solution as filling agent and with the mixed liquor of methyl alcohol, tetrahydrofuran and phosphate aqueous solution as moving phase with 18 silane group silica gel or eight silane group silica gel.The concentration of described phosphate aqueous solution is preferably 0.05wt%～0.25wt%, more preferably 0.07wt%～0.12wt%, more preferably 0.09wt%～0.11wt%.In the mixed liquor of described methyl alcohol, tetrahydrofuran and phosphate aqueous solution, methyl alcohol: tetrahydrofuran: phosphate aqueous solution is by volume measured than being preferably 15～30: 5～15: 60～75, more preferably 15～30: 5～15: 65～70, more preferably 20～25: 8～12: 65～70, more preferably 23: 10: 67.
The detection wavelength that detects described need testing solution use in liquid chromatograph is preferably 330nm～340nm, more preferably 335nm.The number of theoretical plate that detects described need testing solution in liquid chromatograph calculates by the lamp-dish flower acetic peak and preferably is not less than 5000, more preferably is not less than 8000.
According to the present invention, preferably in described liquid chromatograph, inject the lamp-dish flower acetic reference substance solution and detect, obtain the content of lamp-dish flower acetic in the described need testing solution then with calculated by peak area with external standard method.
According to the present invention, the method for quality control of described lamp-dish flower acetic also comprises the step that detects its related substances in the lamp-dish flower acetic, and the step of described detection its related substances specifically comprises:
The related substance inspection need testing solution of lamp-dish flower acetic is provided;
Get described need testing solution dilution and obtain contrast solution;
Get described related substance inspection and in liquid chromatograph, analyze, contrast described related substance inspection the related substance peak area of need testing solution and the main peak area of described contrast solution, obtain the content of described related substance with need testing solution and contrast solution.
That related substance in the lamp-dish flower acetic of the present invention is defined in is close with the lamp-dish flower acetic structure in the lamp-dish flower acetic, and can show the material of impurity peaks in chromatograph.
According to the present invention, in the step that detects its related substances, described related substance inspection is preferably 0.1mg/ml～0.3mg/ml with the concentration of need testing solution, more preferably 0.15mg/ml～0.25mg/ml, more preferably 0.2mg/ml.The concentration of described contrast solution is preferably 2 μ g/ml～30 μ g/ml, more preferably 2 μ g/ml～10 μ g/ml.
According to the present invention, in the step that detects its related substances, the described stationary phase that uses when described contrast solution and need testing solution detect in liquid chromatography of getting is octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels, and moving phase is the mixed liquor of methyl alcohol, tetrahydrofuran and phosphate aqueous solution.The concentration of described phosphate aqueous solution is preferably 0.05wt%～0.25wt%, more preferably 0.07wt%～0.12wt%, more preferably 0.09wt%～0.11wt%.In the mixed liquor of described methyl alcohol, tetrahydrofuran and phosphate aqueous solution, methyl alcohol: tetrahydrofuran: phosphate aqueous solution is by volume measured than being preferably 15～30: 5～15: 60～75, more preferably 15～30: 5～15: 65～70, more preferably 20～25: 8～12: 65～70, more preferably 23: 10: 67.
According to the present invention, in the step that detects the lamp-dish flower acetic its related substances, described to get described contrast solution and the related substance inspection time when analyzing in liquid chromatography with need testing solution be more than 2 times of lamp-dish flower acetic major component peak retention time.Other condition of described liquid chromatograph can be identical with the condition of liquid chromatograph in the described detection lamp-dish flower acetic purity.
According to the present invention, the method for quality control of described lamp-dish flower acetic also comprise with described lamp-dish flower acetic Cu-K α target emanation,
Carry out X-ray diffraction under the condition of 2 θ=2 °～70 ° and detect, confirm whether to possess X-ray diffraction peak as described in Table 1.If described lamp-dish flower acetic has an X-ray diffractogram peak as table 1, show that then described lamp-dish flower acetic has desired crystal structure, if the X-ray diffraction peak of diffraction peak and table 1 is inconsistent, show that then the structure of described lamp-dish flower acetic is different with desired lamp-dish flower acetic crystal structure.
According to the present invention, described method of quality control also comprises described lamp-dish flower acetic is carried out infrared detection, confirms whether described lamp-dish flower acetic has following wave number (cm
-1): 3511 ± 2,3373 ± 2,2920 ± 2,2885 ± 2,1721 ± 2,1662 ± 2,1608 ± 2,1575 ± 2,1498 ± 2,1467 ± 2,1442 ± 2,1400 ± 2,1362 ± 2,1286 ± 2,1249 ± 2,1224 ± 2,1183 ± 2,1150 ± 2,1119 ± 2,1101 ± 2,1084 ± 2,1041 ± 2,846 ± 2,813 ± 2,740 ± 2,720 ± 2,618 ± 2.If described lamp-dish flower acetic has above-mentioned wave number, show that then described lamp-dish flower acetic has desired group, if described lamp-dish flower acetic and above-mentioned wave number are inconsistent, then can determine the different groups of described lamp-dish flower acetic and desired lamp-dish flower acetic, for example the position of some group and desired group position are inconsistent.
According to the present invention, whether the method for quality control of described lamp-dish flower acetic also comprises the step of described lamp-dish flower acetic being carried out differential scanning calorimetric (DSC) analysis, be 124 ℃～128 ℃ to confirm described lamp-dish flower acetic endothermic transition temperature.According to the present invention, the method of quality control of described lamp-dish flower acetic also comprises described lamp-dish flower acetic is carried out thermogravimetric-differential thermal (TGA) analytical procedure, confirming whether described lamp-dish flower acetic fusion and decomposition temperature is 202 ℃～215 ℃, and whether confirm mass attenuation with 12%～15%.By lamp-dish flower acetic being carried out DSC and TGA test, can confirm whether the thermal behavior of described lamp-dish flower acetic is consistent with desired lamp-dish flower acetic thermal behavior, thereby confirm whether lamp-dish flower acetic satisfies the quality requirements of thermal behavior.
The invention provides a kind of method of quality control of lamp-dish flower acetic.In described method of quality control, with octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels is filling agent, mixed liquor with methyl alcohol, tetrahydrofuran and phosphate aqueous solution is a moving phase, detect described need testing solution in liquid chromatograph, external standard method obtains the content of described lamp-dish flower acetic.By described method of quality control, can in preparation lamp-dish flower acetic process, the quality of lamp-dish flower acetic be estimated accurately, to guarantee finally to obtain stay-in-grade lamp-dish flower acetic.
In order further to understand the present invention, be described below in conjunction with the method for quality control of embodiment lamp-dish flower acetic provided by the invention.
Below for the used lamp-dish flower acetic that is numbered 200904-B, 200904-C, 200904-D that provides by Kunming pharmacy group of the embodiment of the invention as three kinds of specimen.
The use instrument is: the LC-10ATVP high performance liquid chromatograph that Tianjin, island (Shimadzu) company produces: comprise that Shimadzu LC-10ATVP pump, FCV-10ALVP+DGU-12A make up online degasser, SIL-10ADVP automatic sampler, SPD-M10AVP diode array detector, CTO-10ASVP column oven, CLASS-VP workstation, chromatographic column are Luna C18150 * 4.6mm.
With 18 silane group silica gel is filling agent, mixed liquor with methyl alcohol-tetrahydrofuran-phosphate aqueous solution is a moving phase, in the described mixed liquor, methyl alcohol by volume: tetrahydrofuran: phosphate aqueous solution is 23: 10: 67, phosphate aqueous solution concentration is 0.1wt%, the detection wavelength is 335nm, and number of theoretical plate is pressed the lamp-dish flower acetic peak and calculated 8000.
Get the specimen that is numbered 200904-B, add dissolve with methanol and dilution obtain concentration be the solution of 50 μ g/ml as need testing solution, measure described need testing solution 10 μ l and inject liquid chromatograph, the record chromatogram, as shown in Figure 1, stratographic analysis result such as table 2:
The stratographic analysis result of table 2, embodiment 1 lamp-dish flower acetic need testing solution
The scutellarin that getting Nat'l Pharmaceutical ﹠ Biological Products Control Institute provides (has another name called lamp-dish flower acetic, lot number 8420-200102) reference substance, add dissolve with methanol and dilute and obtain the solution that concentration is 50 μ g/ml, product solution in contrast, measure described reference substance solution 10 μ l and inject liquid chromatograph, the record chromatogram;
Use the single-point external standard method to calculate content: the ratio of the peak area by calculating described need testing solution and reference substance solution promptly gets the content of described test sample.The result of three kinds of specimen is as follows: 200904-B, 200904-C, 200904-D contain lamp-dish flower acetic by dry product calculating and are respectively 98.0wt%, 99.2wt%, 98.5wt%.
Embodiment 2
Used chromatograph, filling agent, moving phase are identical with embodiment 1.
Get the lamp-dish flower acetic sample, make the need testing solution of 0.2mg/ml with dissolve with methanol; Get the described need testing solution of part and make the reference substance solution of 4 μ g/ml with the methyl alcohol dilution.
Get described reference substance solution 10 μ l and inject liquid chromatograph, regulate detection sensitivity, make the major component peak height be about 10% of record full scale;
Get each 10 μ l of described reference substance solution and need testing solution and inject the liquid chromatograph detection, the record chromatogram is to 2 times of major component peak retention time.
Figure 2 shows that to be numbered 200904-B need testing solution chromatogram, the related substance peak all shows.Table 3 is corresponding stratographic analysis result.
The stratographic analysis result of lamp-dish flower acetic need testing solution among table 3, the embodiment 2
Figure 3 shows that the reference substance solution chromatogram, only shown that main peak, table 4 are corresponding stratographic analysis result:
The stratographic analysis result of contrast solution among table 4, the embodiment 2
Calculate, its related substances is less than 2.0wt% among the sample 200904-B.
Sample 200904-C, 200904-D test result are shown its related substances in above-mentioned two kinds of samples is all less than 4.0wt%.
Embodiment 3
Sample thief 200904-B carries out X-ray analysis:
Instrument: Japanese D/MAX-2200 type diffractometer of science
Target: Cu-K α radiation
2 θ=2 °～70 °
Step angle: 0.04 °
Pipe is pressed: 36KV
Pipe stream: 30mA
Sweep velocity: 10 °/min:
X ray diffracting spectrum is seen shown in Figure 4, result such as table 5:
The X-ray diffraction analysis result of table 5, sample 200904-B
The result of table 5 shows that sample 200904-B has identical crystal structure with desired lamp-dish flower acetic.
Embodiment 4
Sample thief 200904-C carries out infrared spectrum (IR) analysis
Instrument: Shimadzu FTIR-8400S infrared spectrometer
Compressing tablet: pressing potassium bromide troche
Infared spectrum is asked for an interview Fig. 5, infrared spectrum wave number (cm
-1) be: 3511,3373,2920,2885,1721,1662,1608,1590,1575,1558,1498,1467,1442,1418,1400,1362,1304,1286,1249,1224,1198,1183,1150,1119,1101,1084,1041,846,813,740,720,618.
Test result shows that sample 200904-C has the group identical with the lamp-dish flower acetic of described requirement.
Sample thief 200904-C carries out differential scanning calorimetric (DSC) and thermogravimetric-differential thermal (TGA) is analyzed;
Instrument: NETZSCH STA 409 PG/PC
Temperature range: 35～350 ℃
Programming rate: 5 ℃/minute
TG range: ± 250 μ V
Reference substance: Al
2O
3
Temperature range: 35 ℃～350 ℃
As shown in Figure 6, be the DSC-TGA curve of sample described in the present embodiment, from the DSC curve as can be known, the sample melted decomposition temperature is 207 ℃～209 ℃, and the endothermic transition temperature is 124 ℃～128 ℃; From the TGA curve as can be known, the sample melted decomposition temperature is at 202 ℃～215 ℃, and with 12%～15% mass attenuation.
Test result shows that sample 200904-C has shown the fusion and decomposition temperature identical with lamp-dish flower acetic, endothermic transition temperature and thermal weight loss on the DSC-TGA curve, can confirm that it satisfies the thermal behavior quality requirements.
More than the method for quality control that the invention provides lamp-dish flower acetic is described in detail.Used specific case herein principle of the present invention and embodiment are set forth, the explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof.Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of claim of the present invention.
Claims (15)
1. the method for quality control of a lamp-dish flower acetic comprises:
The assay need testing solution of lamp-dish flower acetic is provided;
Be filling agent, be moving phase that with octadecylsilane or eight alkyl silane bonded silica gels detect described need testing solution in liquid chromatograph, the external standard method analysis obtains the content of described lamp-dish flower acetic with the mixed liquor of methyl alcohol, tetrahydrofuran and phosphate aqueous solution.
2. method of quality control according to claim 1 is characterized in that, the concentration of described phosphate aqueous solution is 0.05wt%～0.25wt%.
3. method of quality control according to claim 2 is characterized in that, be methyl alcohol in the mixed solution of described methyl alcohol, tetrahydrofuran and phosphate aqueous solution by volume: tetrahydrofuran: phosphate aqueous solution is 21～25: 8～12: 65～70.
4. method of quality control according to claim 1 is characterized in that, the described number of theoretical plate that detects described need testing solution in liquid chromatograph calculates by the lamp-dish flower acetic peak and is not less than 5000.
5. method of quality control according to claim 1 is characterized in that, the described detection wavelength that the described need testing solution of detection uses in chromatograph is 330nm～340nm.
6. according to each described method of quality control of claim 1 to 5, it is characterized in that also comprise the step that detects its related substances in the described lamp-dish flower acetic, the step of its related substances specifically comprises in the described lamp-dish flower acetic of described detection:
The related substance inspection need testing solution of lamp-dish flower acetic is provided;
Get described need testing solution dilution and obtain contrast solution;
Get described contrast solution and the related substance inspection is analyzed in liquid chromatography with need testing solution, contrast the related substance peak area of described need testing solution and the main peak area of described reference substance solution, obtain the content of described related substance.
7. method of quality control according to claim 6, it is characterized in that, described described contrast solution and the need testing solution got detects the stationary phase that uses and is octadecylsilane chemically bonded silica or eight alkyl silane bonded silica gels in liquid chromatography, moving phase is the mixed liquor of methyl alcohol, tetrahydrofuran and phosphate aqueous solution.
8. method of quality control according to claim 7 is characterized in that, the described time when getting described contrast solution and need testing solution and analyzing in liquid chromatography is more than 2 times of lamp-dish flower acetic major component peak retention time.
9. method of quality control according to claim 8 is characterized in that, in the step of its related substances, the concentration of described need testing solution is 0.1mg/ml～0.3mg/ml in the described lamp-dish flower acetic of described detection.
10. method of quality control according to claim 9 is characterized in that, in the step of its related substances, the concentration of described contrast solution is 2 μ g/ml～10 μ g/ml in the described lamp-dish flower acetic of described detection.
11. method of quality control according to claim 10 is characterized in that, in the described lamp-dish flower acetic of described detection in the step of its related substances, described described contrast solution and the need testing solution got analyzed in liquid chromatography and specifically comprised:
Get described contrast solution and inject liquid chromatograph, make the major component peak height be about 10% of registering instrument full scale;
Get described contrast solution and described need testing solution 5-20 μ l injecting chromatograph, the related substance peak of described need testing solution is all shown.
12. method of quality control according to claim 6 is characterized in that, also comprise with described lamp-dish flower acetic Cu-K α target emanation,
Carry out X-ray diffraction under the condition of 2 θ=2 °～70 ° and detect, confirm whether possess as the described X ray diffracting spectrum of following table:
13. method of quality control according to claim 12 is characterized in that, also comprises described lamp-dish flower acetic is carried out infrared detection, confirms whether to have following wave number (cm
-1): 3511 ± 2,3373 ± 2,2920 ± 2,2885 ± 2,1721 ± 2,1662 ± 2,1608 ± 2,1575 ± 2,1498 ± 2,1467 ± 2,1442 ± 2,1400 ± 2,1362 ± 2,1286 ± 2,1249 ± 2,1224 ± 2,1183 ± 2,1150 ± 2,1119 ± 2,1101 ± 2,1084 ± 2,1041 ± 2,846 ± 2,813 ± 2,740 ± 2,720 ± 2,618 ± 2.
14. whether method of quality control according to claim 13 is characterized in that, also comprises the step of described lamp-dish flower acetic being carried out the differential scanning thermometric analysis, be 124 ℃～128 ℃ to confirm described lamp-dish flower acetic endothermic transition temperature.
15. method of quality control according to claim 14, it is characterized in that, whether, to confirm its fusion and decomposition temperature be 202 ℃～215 ℃, and whether confirm the mass attenuation with 12%～15% if also comprising described lamp-dish flower acetic is carried out thermogravimetric-differential thermal analysis (DTA).
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| CN104483405A (en) * | 2014-12-11 | 2015-04-01 | 云南生物谷药业股份有限公司 | Detection method of related substances in vegetable drug extract-scutellarin |
| CN104597201A (en) * | 2013-10-30 | 2015-05-06 | 昆明制药集团股份有限公司 | Method for detecting scutellarin content |
| CN109470795A (en) * | 2018-12-27 | 2019-03-15 | 云南生物谷药业股份有限公司 | The detection method of content of scutellarin in Chinese medicine |
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| CN103743645A (en) * | 2013-07-19 | 2014-04-23 | 中国石油化工股份有限公司 | Method for controlling quality of polymer for reservoir oil displacement using thermal gravimetric analysis technology |
| CN104597201A (en) * | 2013-10-30 | 2015-05-06 | 昆明制药集团股份有限公司 | Method for detecting scutellarin content |
| CN104483405A (en) * | 2014-12-11 | 2015-04-01 | 云南生物谷药业股份有限公司 | Detection method of related substances in vegetable drug extract-scutellarin |
| CN104483405B (en) * | 2014-12-11 | 2015-10-21 | 云南生物谷药业股份有限公司 | The detection method of the related substances in autonomic drug extract lamp-dish flower acetic |
| CN109470795A (en) * | 2018-12-27 | 2019-03-15 | 云南生物谷药业股份有限公司 | The detection method of content of scutellarin in Chinese medicine |
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Application publication date: 20110420 |