CN105954431B - A kind of method of the HPLC separation determination Ao Pei meter Fen bulk pharmaceutical chemicals in relation to substance - Google Patents
A kind of method of the HPLC separation determination Ao Pei meter Fen bulk pharmaceutical chemicals in relation to substance Download PDFInfo
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- CN105954431B CN105954431B CN201610544063.2A CN201610544063A CN105954431B CN 105954431 B CN105954431 B CN 105954431B CN 201610544063 A CN201610544063 A CN 201610544063A CN 105954431 B CN105954431 B CN 105954431B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
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Abstract
The present invention relates to a kind of with method of the HPLC separation determination Ao Pei meter Fen bulk pharmaceutical chemicals in relation to substance, include the following steps：Using octadecylsilane chemically bonded silica as filler, it is mobile phase A using phosphoric acid water transfer pH to 2.5~3.5, methanol acetonitrile carries out gradient elution as Mobile phase B, flow velocity is 0.8~1.2mL/min, and column temperature is 32~37 DEG C, and the related substance of Ao Pei meter Fen bulk pharmaceutical chemicals is detected using UV detector.The method of the present invention has the advantages that fast and convenient, high sensitivity, accurately and reliably, suitable for the related substance of separation determination Ao Pei meter Fen bulk pharmaceutical chemicals.The method of the present invention is by considering analytical column, mobile phase, gradient elution program and flow velocity, column temperature to the combined influence of separation detection, so that testing result has reached optimization, there is fast and convenient, high sensitivity, accurately and reliably, suitable for the related substance of separation determination Ao Pei meter Fen bulk pharmaceutical chemicals.
Description
Technical field
The present invention relates to a kind of analysis determining methods of Ao Pei meter Fen bulk pharmaceutical chemicals, and in particular to a kind of to use HPLC separation determinations
Method of the Ao Pei meter Fen bulk pharmaceutical chemicals in relation to substance.
Background technology
Ao Pei meter Fen is a kind of estrogen-agonistic medicine and antagonistic with tissue selectivity effect.The medicine to estrogen by
Body α's (ER α) and β (ER β) is affinity.Its biological action is by being combined mediation with estrogen receptor.Such combination
Cause the activation (agonism) of the estrogen pathway in some tissues and block other estrogen pathway (antagonism), molecule
Formula is C24H23ClO2, molecular weight 378.9, structural formula is as follows：
In order to control the quality of Ao Pei meter Fen bulk pharmaceutical chemicals, it is necessary to control main component and impurity, in existing skill
In art, quick, easy, Accurate Analysis detection analysis method of the Ao Pei meter Fen bulk pharmaceutical chemicals in relation to substance it is not suitable for.
Therefore, there is further improvement and optimization demand for assay method of the Ao Pei meter Fen bulk pharmaceutical chemicals in relation to substance,
This is exactly the power that the present invention is accomplished and starting point place.
The content of the invention
In order to overcome above-mentioned technical problem existing in the prior art, the present inventor is carrying out substantial amounts of further investigation
Afterwards, so as to provide a kind of method of the HPLC separation determination Ao Pei meter Fen bulk pharmaceutical chemicals in relation to substance, have fast and convenient, sensitive
Degree is high, accurately and reliably the advantages of.
The invention is realized by the following technical scheme, in particular to a kind of former with HPLC separation determinations Ao Pei meter Fen
Expect method of the medicine in relation to substance, include the following steps：Using octadecylsilane chemically bonded silica as filler, with phosphoric acid water transfer pH extremely
2.5~3.5 be mobile phase A, methanol-acetonitrile is that Mobile phase B carries out gradient elution, and flow velocity is 0.8~1.2mL/min, and column temperature is
32~37 DEG C, the related substance of Ao Pei meter Fen bulk pharmaceutical chemicals is detected using UV detector.
Preferably, the grain size of the octadecylsilane chemically bonded silica is 5 μm, column internal diameter 4.6mm, column length 250mm.
Preferably, it is mobile phase A with phosphoric acid water transfer pH to 3.0.
Preferably, in the Mobile phase B, the volume ratio of methanol and acetonitrile is 30: 70.
Preferably, in gradient elution, flow velocity 1.0mL/min, column temperature is 35 DEG C.
Preferably, the detailed process of the gradient elution is：
Preferably, the Detection wavelength of the UV detector is 230nm.
Compared with prior art, beneficial effects of the present invention are as follows：The method of the present invention is by considering analytical column, flowing
Phase, gradient elution program and flow velocity, column temperature are to the combined influence of separation detection so that testing result has reached optimization, tool
Have fast and convenient, high sensitivity, accurately and reliably the advantages of, suitable for the related substance of separation determination Ao Pei meter Fen bulk pharmaceutical chemicals.
Description of the drawings
Fig. 1 is liquid phase spectrograms of the Ao Pei meter Fen in relation to substance.
Specific embodiment
With reference to specific embodiment, the present invention is described in detail.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill to this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection domain.
A kind of method of the HPLC separation determination Ao Pei meter Fen bulk pharmaceutical chemicals in relation to substance, includes the following steps：With octadecane
Base silane bonded silica gel is filler, and the grain size of octadecylsilane chemically bonded silica is 5 μm, column internal diameter 4.6mm, and column length is
250mm using phosphoric acid water transfer pH to 3.0 is mobile phase A, volume ratio as 30: 70 methanol-acetonitrile is mobile phase, carries out gradient and washes
De-, gradient elution program is shown in Table 1, and flow velocity 1.0mL/min, column temperature is 35 DEG C, using UV detector to Ao Pei meter Fen raw materials
The related substance of medicine is detected, and the liquid phase spectrogram of Detection wavelength 230nm, Ao Pei meter Fen bulk pharmaceutical chemicals sample is as shown in Figure 1, Austria
The peak value of Pei meter Fen bulk pharmaceutical chemicals samples is as shown in table 2.
1 gradient elution program of table
| Time (minute) | Mobile phase A (volume %) | Mobile phase B (volume %) |
| 0 | 50 | 50 |
| 8 | 50 | 50 |
| 12 | 35 | 65 |
| 35 | 25 | 75 |
| 60 | 10 | 90 |
| 60.1 | 50 | 50 |
| 70 | 50 | 50 |
The peak value meter of 2 Ao Pei meter Fen bulk pharmaceutical chemicals of table
| It numbers at peak | Retention time min | Height mAu | Area mAu*s | Area % | Tailing factor | Theoretical cam curve | Separating degree |
| A | 8.065 | 15.95 | 216.87 | 0.745 | 0.903 | 7519 | |
| B | 8.679 | 19.75 | 274.91 | 0.945 | 0.949 | 8746 | 1.6 |
| C | 12.498 | 18.32 | 267.33 | 0.919 | 0.969 | 15898 | 9.9 |
| D | 14.119 | 16.20 | 210.39 | 0.723 | 0.891 | 27612 | 4.4 |
| E | 18.060 | 16.64 | 208.82 | 0.718 | 0.973 | 45172 | 11.6 |
| F | 30.086 | 20.11 | 314.15 | 1.079 | 1.017 | 83924 | 31.8 |
| Main ingredient | 31.179 | 1681.74 | 27109.74 | 93.147 | 1.048 | 85837 | 2.6 |
| G | 32.075 | 14.30 | 239.60 | 0.823 | 0.933 | 85762 | 2.1 |
| H | 34.090 | 15.39 | 262.60 | 0.902 | 1.030 | 90517 | 4.5 |
System suitability：Take Ao Pei meter Fen and impurity A, B, C, D, E, F, G, H reference substance appropriate respectively, precision claims
It is fixed, it puts in same volumetric flask, adds methanol appropriate, ultrasound makes dissolving and dilute be made in every 1mL containing about Ao Pei meter Fen 0.5mg, contain
Each impurity is about the mixed solution of 5 μ g, and each peak separating degree should be not less than 1.5.
Specific test operation：Take this product appropriate, methanol is added to dissolve and quantify dilution be made it is molten containing about 0.5mg in every 1mL
Liquid measures 1mL, puts in 100mL measuring bottles, scale is diluted to solvent, as contrast solution as test solution, precision.It takes pair
Inject liquid chromatograph according to 20 μ L of solution, adjust detection sensitivity, make the peak height of principal component chromatographic peak for full scale 10%~
20%.It is accurate again to measure test solution and each 20 μ L of contrast solution, liquid chromatograph is injected separately into, records chromatogram.For examination
If any impurity peaks in the chromatogram of product solution, single impurity peak area is not greater than 0.10 times of contrast solution main peak area
(0.10%), the sum of each impurity peak area is not greater than 1.0 times (1.0%) of the main peak area of contrast solution.It is (impurity C, miscellaneous
Matter D, impurity E correction factor are respectively 0.74,0.80,0.80；Remaining known impurities and unknown impuritie correction factor are based on 1.0
It calculates).
Calculation formula：
Total miscellaneous content=Σ known impurity level+Σ other impurities contents
AIt is single：Impurity peak area AControl：1% control main peak area F：Correction factor
| Impurity title | Relative retention time | Correction factor (F) |
| Impurity A | 0.26 | 0.92 |
| Impurity B | 0.28 | 1.06 |
| Impurity C | 0.40 | 0.74 |
| Impurity D | 0.45 | 0.80 |
| Impurity E | 0.58 | 0.80 |
| Impurity F | 0.96 | 1.00 |
| Impurity G | 1.03 | 0.92 |
| Impurity H | 1.09 | 1.04 |
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substantive content of the present invention.
Claims (5)
1. a kind of method of the HPLC separation determination Ao Pei meter Fen bulk pharmaceutical chemicals in relation to substance, which is characterized in that include the following steps：
Using octadecylsilane chemically bonded silica as filler, using phosphoric acid water transfer pH to 2.5~3.5 be mobile phase A, methanol-acetonitrile is stream
Dynamic phase B carries out gradient elution, and flow velocity is 0.8~1.2mL/min, and column temperature is 32~37 DEG C, using UV detector to Ao Pei meter
The related substance of fragrant bulk pharmaceutical chemicals is detected；In the Mobile phase B, the volume ratio of methanol and acetonitrile is 30: 70；The gradient is washed
De- detailed process is：
2. method of the HPLC separation determination Ao Pei meter Fen bulk pharmaceutical chemicals in relation to substance is used as described in claim 1, which is characterized in that
The grain size of the octadecylsilane chemically bonded silica is 5 μm, column internal diameter 4.6mm, column length 250mm.
3. method of the HPLC separation determination Ao Pei meter Fen bulk pharmaceutical chemicals in relation to substance is used as described in claim 1, which is characterized in that
It is mobile phase A with phosphoric acid water transfer pH to 3.0.
4. method of the HPLC separation determination Ao Pei meter Fen bulk pharmaceutical chemicals in relation to substance is used as described in claim 1, which is characterized in that
In gradient elution, flow velocity 1.0mL/min, column temperature is 35 DEG C.
5. method of the HPLC separation determination Ao Pei meter Fen bulk pharmaceutical chemicals in relation to substance is used as described in claim 1, which is characterized in that
The Detection wavelength of the UV detector is 230nm.
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| CN201610544063.2A CN105954431B (en) | 2016-07-11 | 2016-07-11 | A kind of method of the HPLC separation determination Ao Pei meter Fen bulk pharmaceutical chemicals in relation to substance |
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| CN105954431B true CN105954431B (en) | 2018-05-29 |
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