CN107192773B - A kind of detection is difficult to understand uncommon for Buddhist nun's content and the high-efficient liquid phase technique in relation to substance - Google Patents
A kind of detection is difficult to understand uncommon for Buddhist nun's content and the high-efficient liquid phase technique in relation to substance Download PDFInfo
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- CN107192773B CN107192773B CN201710347869.7A CN201710347869A CN107192773B CN 107192773 B CN107192773 B CN 107192773B CN 201710347869 A CN201710347869 A CN 201710347869A CN 107192773 B CN107192773 B CN 107192773B
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- 238000001514 detection method Methods 0.000 title claims abstract description 23
- 239000000126 substance Substances 0.000 title abstract description 13
- 238000000034 method Methods 0.000 title description 6
- 239000007791 liquid phase Substances 0.000 title description 4
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 239000008363 phosphate buffer Substances 0.000 claims abstract description 9
- FGDQGIKMWOAFIK-UHFFFAOYSA-N acetonitrile;phosphoric acid Chemical compound CC#N.OP(O)(O)=O FGDQGIKMWOAFIK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- 239000012535 impurity Substances 0.000 claims description 16
- 239000012085 test solution Substances 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 14
- 238000012360 testing method Methods 0.000 claims description 14
- 239000013558 reference substance Substances 0.000 claims description 11
- 239000012086 standard solution Substances 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 8
- 238000005259 measurement Methods 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 7
- 238000004090 dissolution Methods 0.000 claims description 5
- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 2
- 238000010828 elution Methods 0.000 claims 2
- 238000011095 buffer preparation Methods 0.000 claims 1
- 239000000945 filler Substances 0.000 claims 1
- 238000002360 preparation method Methods 0.000 claims 1
- 239000012087 reference standard solution Substances 0.000 claims 1
- 239000000523 sample Substances 0.000 claims 1
- 238000005220 pharmaceutical analysis Methods 0.000 abstract description 2
- 239000012071 phase Substances 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 4
- 206010058467 Lung neoplasm malignant Diseases 0.000 description 2
- 241000594182 Sarcophaga sigma Species 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000010829 isocratic elution Methods 0.000 description 2
- 201000005202 lung cancer Diseases 0.000 description 2
- 208000020816 lung neoplasm Diseases 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 230000001394 metastastic effect Effects 0.000 description 2
- 206010061289 metastatic neoplasm Diseases 0.000 description 2
- 230000035772 mutation Effects 0.000 description 2
- 239000006187 pill Substances 0.000 description 2
- 102200048955 rs121434569 Human genes 0.000 description 2
- 229940121358 tyrosine kinase inhibitor Drugs 0.000 description 2
- 239000005483 tyrosine kinase inhibitor Substances 0.000 description 2
- 150000004917 tyrosine kinase inhibitor derivatives Chemical class 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 238000002965 ELISA Methods 0.000 description 1
- 206010027476 Metastases Diseases 0.000 description 1
- 108091000080 Phosphotransferase Proteins 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 210000004556 brain Anatomy 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- RVRCFVVLDHTFFA-UHFFFAOYSA-N heptasodium;tungsten;nonatriacontahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[W].[W].[W].[W].[W].[W].[W].[W].[W].[W].[W] RVRCFVVLDHTFFA-UHFFFAOYSA-N 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000009401 metastasis Effects 0.000 description 1
- 208000002154 non-small cell lung carcinoma Diseases 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 102000020233 phosphotransferase Human genes 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
Classifications
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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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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Investigating Or Analysing Biological Materials (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The present invention relates to a kind of Pharmaceutical Analysis fields, and in particular to a kind of detection is difficult to understand uncommon for Buddhist nun's content and the high performance liquid chromatography in relation to substance.Chromatographic condition is using U.S. Agilent high performance liquid chromatograph, Agilent Eclipse Plus chromatographic column C18(5 μm of 250 × 4.6mm), mobile phase is with acetonitrile-phosphate buffer (6.8gKH2PO4It is dissolved in 1L water, H3PO4Adjust pH=2.8)=27:73, Detection wavelength 272nm, flow velocity 1ml/min, sample volume is 5 μ l.The detection method is accurate and reliable, chromatographic peak good separating effect, can efficient detection Austria is uncommon replaces Buddhist nun's content and related substance.
Description
Technical field
It is difficult to understand uncommon for Buddhist nun's content and in relation to the high performance liquid chromatography of substance that the present invention relates to a kind of detections, belongs to Pharmaceutical Analysis
Field.
Technical background
Ao Xi replaces Buddhist nun (structural formula is shown in attached drawing 1) molecular formula: C28H33N7O2·CH4O3S, yellow crystalline powder.For treating
The targeted drug of EGFR T790M mutation positive Locally Advanced or Metastatic Nsclc.It is a kind of oral kinases
Inhibitor, for previously going out through when EGF-R ELISA (EGFR) tyrosine kinase inhibitor (TKI) is treated or after treatment
Existing progression of disease, and the Locally Advanced or metastatic non-cellule type positive there are EGFR T790M mutation through detection confirmation
The treatment of lung cancer (NSCLC) adult patient, and have research that there is significant treatment in brain metastasis.In China, annual new hair
The patients with lung cancer of disease is more than 730,000 people, is the highest malignant tumour of morbidity and mortality.Contain at present about detection west difficult to understand for Buddhist nun
It is not studied in terms of amount and related substance.Content and related object with regard to this present invention using high-efficient liquid phase technique detection west difficult to understand for Buddhist nun
Matter, with acetonitrile-phosphate buffer (6.8gKH2PO4It is dissolved in 1L water, H3PO4Adjust pH=2.8) it is mobile phase, isocratic elution.
The detection method simple and effective, chromatographic peak separating degree is fine, and separating degree is greater than 1.5, meets 2010 editions examination criterias of Chinese Pharmacopoeia,
And chromatographic peak without trail it is unmatched prolong phenomenon, tailing factor T=1.12 meets 2010 editions regulation tailing factors 0.95 of Chinese Pharmacopoeia
~1.05.So the detection method has important application value with impurity analysis in uncommon control for Buddhist nun's content of Austria.
Summary of the invention
It is difficult to understand uncommon for Buddhist nun's content and related substance that the present invention through multiple microtest provides a kind of more acurrate, efficient measurement
High performance liquid chromatography.For the attainment of one's purpose, the following technical solution of the present invention:
In a specific embodiment of the invention, the present invention is difficult to understand uncommon for Buddhist nun using the measurement of Agilent high performance liquid chromatograph
Content and related substance, with acetonitrile-phosphate buffer (6.8gKH2PO4It is dissolved in 1L water, H3PO4Adjust pH=2.8) it is stream
It is dynamic mutually to carry out isocratic elution, and verified by many experiments, the preferred 27:73 of mobile phase ratio.
In another specific embodiment of the invention, the present invention provides Agilent Eclipse Plus octadecyl bonded silica
Glue chromatographic column or the comparable chromatographic column of efficiency, are verified by many experiments, the preferred Agilent Eclipse Plus of the present invention
Chromatographic column, analysis chromatographic peak profile is preferable, and no tailing peak is without leading peak.
In another of the invention specific embodiment, octadecyl silane chromatograph packing material particle is 3-5 μm, preferably 5 μm,
The length of chromatographic column is 150mm or 250mm, preferably 250mm.
In another specific embodiment of the invention, 190nm-400nm full wavelength scanner is carried out using DAD detector, as a result
Ao Xi has absorption maximum for Buddhist nun at 212nm, 272nm, 374nm, and the uncommon related substance for replacing Buddhist nun difficult to understand also has under 272nm wavelength
It is preferable to absorb, therefore preferably 272nm is uncommon for Buddhist nun's content and in relation to the Detection wavelength of substance-measuring as Austria.
In another specific embodiment of the invention, determine that sample volume, sample introduction are accurate using the multiple sample introduction of standard solution
Spending number is 5 times, and the best sample volume of gained is 5 μ l.
For the present invention there are one in specific embodiment, the flow velocity of the mobile phase is 0.5~1.2ml/min, preferably 1ml/
min。
The present invention provides a kind of HPLC method measurement Austria and wishes for Buddhist nun's content and the method in relation to substance, and its step are as follows:
Standard solution is prepared: taking difficult to understand wish to replace Buddhist nun's standard items appropriate, with methanol dissolution and constant volume, compound concentration 1.5mg/
The standard solution of ml.
Test solution is prepared: taking the Austria in laboratory uncommon appropriate for Buddhist nun, with methanol dissolution and constant volume, compound concentration are
The test solution of 1.5mg/ml.
Reference substance solution is prepared: taking above-mentioned difficult to understand wish to be placed in 25ml volumetric flask for Buddhist nun's standard solution 1ml, simultaneously with methanol dilution
Constant volume, compound concentration are the reference substance solution of 0.06mg/ml.
Detailed description of the invention
Fig. 1 is difficult to understand uncommon for Buddhist nun's structural formula
Fig. 2 is difficult to understand uncommon for Buddhist nun's test sample liquid chromatogram
Fig. 3 is difficult to understand uncommon for Buddhist nun's standard items liquid chromatogram
Fig. 4 is difficult to understand uncommon for Buddhist nun's reference substance liquid chromatogram
Fig. 5 is difficult to understand uncommon for Buddhist nun's Detection wavelength liquid chromatogram
Embodiment
Chromatographic condition:
Using U.S.'s Agilent high performance liquid chromatograph, Agilent Eclipse Plus chromatographic column C18(250×4.6mm
5 μm), mobile phase is with acetonitrile-phosphate buffer (6.8gKH2PO4It is dissolved in 1L water, H3PO4Adjust pH=2.8)=27:73, inspection
Survey wavelength is 272nm, and flow velocity 1ml/min, sample volume is 5 μ l.
Above-mentioned test solution and standard solution are taken respectively, inject liquid chromatograph, chromatographic condition according to the invention
It is measured, content 1 calculates as follows:
Ao Xi replaces Buddhist nun's content (%)=(A1 × C2)/(A2 × C1)
Wherein, A1 is test sample peak area
A2 is standard items peak area
C1 is test sample concentration (mg/ml)
C2 is standard concentration (mg/ml).
Above-mentioned test solution and control solution are taken respectively, inject liquid chromatograph, chromatographic condition according to the invention
It is measured, test sample 2 calculates as follows if any impurity peaks, impurity:
Ao Xi replaces the related content of material of Buddhist nun (%)=(A × 1 × 10 × W2)/(B × 10 × 200 × W1)
Wherein, A is the peak area of impurity peaks in test solution
B is the peak area that Ao Xi replaces Buddhist nun in reference substance solution
W1 is quality when preparing the uncommon weighing for Buddhist nun's test solution difficult to understand
W2 is quality when preparing the uncommon weighing for Buddhist nun's reference substance solution difficult to understand.
Embodiment 1
Experimental material: it is 99.2% that difficult to understand wish for Buddhist nun's test sample content has been demarcated in laboratory by our company, and miscellaneous list is 0.19%, always
Miscellaneous is 0.36%, and Austria is uncommon to be purchased from U.S. sigma company, content 99.0% for Buddhist nun's standard items.
Chromatographic condition: U.S. Agilent high performance liquid chromatograph, Agilent Eclipse Plus chromatographic column C are used18
(250 × 4.6mm5 μm), mobile phase is with acetonitrile-phosphate buffer (6.8gKH2PO4It is dissolved in 1L water, H3PO4Adjust pH=2.8)
=27:73, Detection wavelength 272nm, flow velocity 1ml/min, sample volume are 5 μ l.
Experimental procedure:
Take laboratory Austria, our company uncommon appropriate for Buddhist nun, with methanol dissolution and constant volume, compound concentration is the Ao Xi of 1.5mg/ml
For Buddhist nun's test solution, test solution is prepared 3 times in parallel.
The Austria for taking medicine inspecting institute to buy is uncommon appropriate for Buddhist nun's standard items, with methanol solution and constant volume, compound concentration 1.5mg/ml
Austria it is uncommon replace Buddhist nun's standard solution, standard solution is prepared 3 times in parallel.
Take above-mentioned test solution and control solution respectively, inject liquid chromatograph, according to chromatographic condition of the present invention into
Row detects and records data, wherein same standard items repeat sample introduction 6 times, peak area obtained by test solution and control solution is pressed
Above-mentioned content calculation formula 1 calculates the content that Ao Xi in test sample replaces Buddhist nun.
Fig. 2 is that test sample Austria wishes the chromatogram for replacing Buddhist nun, and it is 6.21min that Austria, which wishes for Buddhist nun's main peak retention time, is divided in test sample
Separate out 3 impurity peaks, retention time 4.02min, 4.38min and 8.87min, 3 impurity peaks be respectively 1.63 from degree,
6.1 and 7.6, good separation (being all larger than 1.5) meets the standard of 2010 editions Chinese Pharmacopoeias.Wherein the impurity of 4.38min is pure
Degree is 0.035%, below lower than 0.1% according to analysis processing standard purity, its content can be neglected.Fig. 3 is standard items
Ao Xi replaces the chromatogram of Buddhist nun, and it is 0.36% that standard solution, which is repeated 6 gained peak area RSD values of sample introduction, it is seen that the detection side
Method repeatability is good.3 sample peak area averages of test sample and standard items are respectively 8092.66 and 8061.79, are contained by above-mentioned
It is 99.38% that amount, which calculates public affairs 1 and calculates our company laboratory Austria and wish for Buddhist nun's content, calculated result such as the following table 1.
1 test sample Austria of table is uncommon to replace Buddhist nun's content detection result such as following table
The result shows that the detection method testing result for Buddhist nun's content difficult to understand uncommon it is accurate, it is reliable, can be used for it is difficult to understand uncommon for Buddhist nun's bulk pharmaceutical chemicals
Or pill content detection and impurity analysis.
Embodiment 2
Experimental material: it is 99.2% that difficult to understand wish for Buddhist nun's test sample content has been demarcated in laboratory by our company, and miscellaneous list is 0.19%, always
Miscellaneous is 0.36%, and Austria is uncommon to be purchased from U.S. sigma company, content 99.0% for Buddhist nun's standard items.
Chromatographic condition: U.S. Agilent high performance liquid chromatograph, Agilent Eclipse Plus chromatographic column C are used18
(250 × 4.6mm5 μm), mobile phase is with acetonitrile-phosphate buffer (6.8gKH2PO4It is dissolved in 1L water, H3PO4Adjust pH=2.8)
=27:73, Detection wavelength 272nm, flow velocity 1ml/min, sample volume are 5 μ l.
Experimental procedure:
The reference substance solution that test solution in Example 1 and above-mentioned concentration are 0.06mg/ml respectively, injects liquid phase
In chromatograph, the peak area of impurity in test solution is measured and recorded according to chromatographic condition of the present invention, by above-mentioned calculating
Formula 2 calculates the uncommon impurity content for Buddhist nun difficult to understand.
Fig. 4 is reference substance solution chromatogram, and wherein test solution impurity peak area is respectively 14.98 and 11.64, control
Product solution peak area is 304.51, and impurity peak area in test solution and reference substance peak area are substituted into formula and calculated, two
Impurity content is respectively 0.19% and 0.15%, and always miscellaneous is 0.34%.
The result shows that the present invention provide it is difficult to understand uncommon it is accurate for detection method result of the Buddhist nun in relation to substance, reliable, can be used for Ao Xi
For the control of the impurity content of Buddhist nun's bulk pharmaceutical chemicals or pill and impurity analysis.
Claims (4)
1. a kind of measurement is difficult to understand uncommon for Buddhist nun and the high performance liquid chromatography in relation to content of material, which is characterized in that the detection method
It is as follows:
Standard solution is prepared: taking difficult to understand wish to replace Buddhist nun's standard items appropriate, with methanol dissolution and constant volume, compound concentration is 1.5mg/ml's
Standard solution；
Test solution is prepared: taking laboratory Austria uncommon appropriate for Buddhist nun, with methanol dissolution and constant volume, compound concentration is 1.5mg/ml's
Test solution；
Reference substance solution is prepared: being taken difficult to understand wish to be placed in 25ml volumetric flask for Buddhist nun's standard solution 1ml, is with methanol dilution and constant volume
The reference substance solution of 0.06mg/ml；
Chromatographic condition: U.S.'s Agilent high performance liquid chromatograph, Agilent Eclipse Plus C18Chromatographic column, in chromatographic column
Diameter is 4.6mm, and column's length is 150mm or 250mm, and the partial size of octadecyl silane chromatographic column filler is 3-5 μm, stream
The elution ratio of dynamic phase acetonitrile-phosphate buffer is 20:80,25:75,27:73 or 30:70, and sample volume is 5-20 μ l；The stream
Phosphate buffer preparation condition is to weigh 6.8gKH in dynamic phase2PO4It is dissolved in 1L water, H3PO4Adjust pH=2.8；
Chromatographic peak measurement: injecting liquid chromatograph for the test sample, reference substance and standard solution of preparation, recording detection data,
And calculate content and impurity content that Ao Xi in test sample replaces Buddhist nun.
2. a kind of measurement as described in claim 1 is difficult to understand uncommon for Buddhist nun and the high performance liquid chromatography in relation to content of material, feature
Be: the elution ratio of the mobile phase acetonitrile-phosphate buffer is 27:73.
3. a kind of measurement as described in claim 1 is difficult to understand uncommon for Buddhist nun and the high performance liquid chromatography in relation to content of material, feature
Be: the chromatographic column specification is 250 × 4.6mm, and partial size is 5 μm.
4. a kind of measurement as described in claim 1 is difficult to understand uncommon for Buddhist nun and the high performance liquid chromatography in relation to content of material, feature
It is: the 5 μ l of sample volume.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710347869.7A CN107192773B (en) | 2017-05-17 | 2017-05-17 | A kind of detection is difficult to understand uncommon for Buddhist nun's content and the high-efficient liquid phase technique in relation to substance |
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| CN201710347869.7A CN107192773B (en) | 2017-05-17 | 2017-05-17 | A kind of detection is difficult to understand uncommon for Buddhist nun's content and the high-efficient liquid phase technique in relation to substance |
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| CN107192773A CN107192773A (en) | 2017-09-22 |
| CN107192773B true CN107192773B (en) | 2019-09-27 |
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| CN107727773B (en) * | 2017-11-23 | 2020-08-18 | 中山奕安泰医药科技有限公司 | Method for detecting purity of oxitinib mesylate by adopting liquid chromatography |
| CN110376309A (en) * | 2019-08-15 | 2019-10-25 | 重庆化工职业学院 | A method of replacing the related substance of Buddhist nun in measurement west difficult to understand |
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| CN106543060A (en) * | 2016-10-31 | 2017-03-29 | 湖南欧亚生物有限公司 | It is a kind of it is difficult to understand this for Buddhist nun's mesylate preparation method |
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