CN107167524A - Method of the gas chromatography separation detection Aripiprazole about material - Google Patents
Method of the gas chromatography separation detection Aripiprazole about material Download PDFInfo
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- CN107167524A CN107167524A CN201710187436.XA CN201710187436A CN107167524A CN 107167524 A CN107167524 A CN 107167524A CN 201710187436 A CN201710187436 A CN 201710187436A CN 107167524 A CN107167524 A CN 107167524A
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- Prior art keywords
- aripiprazole
- chloroethyls
- amine hydrochlorate
- solution
- isosorbide
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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
Abstract
The invention belongs to analytical chemistry field, the invention discloses one kind relevant material two of gas chromatography quick separating detection Aripiprazole（2 chloroethyls）The method of amine hydrochlorate and Isosorbide-5-Nitrae dibromobutane, this method uses methyl polysiloxane class middle polarity capillary chromatographic column, and flame ionization ditector can be quantitative determined two in Aripiprazole（2 chloroethyls）The content of amine hydrochlorate and Isosorbide-5-Nitrae dibromobutane, so as to reach effective control to Aripiprazole purity, realizes the quality controllable of Aripiprazole.The inventive method specificity is strong, and the degree of accuracy is high, and durability is good and easy to operate.
Description
Technical field
The invention belongs to analytical chemistry field, and in particular to the relevant material two of gas chromatography separation determination Aripiprazole
（2- chloroethyls）The method of amine hydrochlorate and 1,4- dibromobutanes.
Background technology
Aripiprazole is a kind of new atypia antipsychotic drug, has bidirectional modulation to DA nervous systems
Effect, is the stabilizer of DA mediators.There is very high affinity with D2, D3,5-HT1A and 5-HT2A acceptor.By to D2 and 5-
The partial agonist of HT1A acceptors acts on and the antagonism of 5-HT2A acceptors is produced antipsychotic effect.Aripiprazole
There are obvious curative effects to schizoid positive and negative symptoms, can also improve the affective symptom occurred together, reduce schizophrenia
The recurrence rate of disease.Aripiprazole chemistry is entitled：7- { 4- [4- (2,3- dichlorophenyl)-l- piperazinyls] butoxy } -3,4- dihydros -
2 (1H)-quinolinones, molecular formula is C23H27N3O2Cl2, structural formula is：
。
The adverse reaction that medicine is produced in Clinical practice is relevant except the pharmacological activity with medicine in itself, sometimes with medicine
Present in impurity also have much relations, to ensure the quality and safety of medicine, register the requirements for pharmaceuticals declared to its technique
During the impurity that introduces carry out research and effectively control.The relevant material introduced in synthesis Aripiprazole technique has two（2- chlorine
Ethyl）Amine hydrochlorate, its molecular formula is C4H10Cl3N, structural formula is：
。
The molecular formula of 1,4- dibromobutanes is C4H8Br2 , structural formula is：
。
Suitable analysis method is selected, relevant material two in Aripiprazole is separated and determine exactly（2- chloroethyls）Amine salt
Hydrochlorate and Isosorbide-5-Nitrae-dibromobutane, to improving Aripiprazole quality, ensureing that drug safety has great importance.
The content of the invention
It is an object of the invention to provide the organic impurities two introduced in a kind of separation detection synthesis Aripiprazole technique（2-
Chloroethyl）The method of amine hydrochlorate and Isosorbide-5-Nitrae-dibromobutane, so as to reach effective control to Aripiprazole purity, it is ensured that A Li
The quality and drug safety of piperazine azoles.
A kind of separation of the present invention, measure Aripiprazole, about the method for material, are to use gas chromatographic analysis skill
Art, is dissolved sample from suitable solvent, according to the formation and physic-chemical property of material to be analyzed, from methyl polysiloxane class
Chromatographic column and flame ionization ditector.
Above-mentioned described solvent can be the one or more in ethanol, methanol, dichloromethane or dimethyl sulfoxide (DMSO).
Above-mentioned described chromatographic column is selected from the brands such as Agilent, Supelco, Phenomenex or Restek.
Above-mentioned described chromatographic column is the polysiloxane-based capillary chromatographic column of middle grade.
Method of separating and assaying of the present invention, can be realized in accordance with the following methods：
1）Take Aripiprazole appropriate, plus the solution of the 100mg containing Aripiprazole in every 1ml is made in absolute ethyl alcohol dissolving, as trying
Product solution；Separately take two（2- chloroethyls）Amine hydrochlorate and Isosorbide-5-Nitrae-appropriate dibromobutane, plus absolute ethyl alcohol dissolving are made in every 1ml and contained
Two（2- chloroethyls）The solution of amine hydrochlorate and each 5 μ g of Isosorbide-5-Nitrae-dibromobutane, is used as reference substance solution；
2）It is 200 ~ 250 DEG C to set injector temperature, and flow rate of carrier gas is 1.0 ~ 3.5ml/min, programmed temperature method, and heating schedule is
135 °C of initial temperature, 1 ~ 3min of constant temperature, with 8 ~ 15 °C per minute of heating rate to 160 °C, 2 ~ 5min of constant temperature, detector temperature
Spend for 250 ~ 300 DEG C, split ratio is 2:1~10:1；
3）Take 1）Middle need testing solution and each 1~3 μ l of reference substance solution, by 2）Chromatographic condition, inject gas chromatograph, use
External standard method is calculated two in Aripiprazole（2- chloroethyls）The content of amine hydrochlorate and 1,4- dibromobutanes.
Wherein：The model of gas chromatograph, has no special requirements, and the gas chromatograph that the present invention is used is Shimadzu（2010
plus）Gas chromatograph；
Detector：Flame ionization ditector；
Chromatographic column：ZB-50 capillary chromatographic columns（60m × 0.32mm, 0.50 μm）；
Injector temperature：200℃；
Detector temperature：250℃；
Carrier gas（Nitrogen）Flow velocity：3.0ml/min；
Split ratio：2:1；
Sampling volume：1μl.
Column temperature rise program：
。
The present invention uses gas chromatography, from methyl polysiloxane class middle polarity capillary chromatographic column（60m×
0.32mm, 0.50 μm）, can be fast and effeciently two in separation determination Aripiprazole（2- chloroethyls）Amine hydrochlorate and 1,4- dibromo fourths
Alkane, solves the relevant material two introduced in synthesis Aripiprazole technique（2- chloroethyls）Amine hydrochlorate and 1,4- dibromobutanes
Separation determination problem, so as to reach effective control to Aripiprazole purity.As a result accompanying drawing 1 ~ 6 is seen.
Brief description of the drawings
Fig. 1：Solvent during embodiment 1（Absolute ethyl alcohol）Gas chromatogram；
Fig. 2：The gas chromatogram of Aripiprazole during embodiment 1；
Fig. 3：Two during embodiment 1（2- chloroethyls）The gas chromatogram of amine hydrochlorate and 1,4- dibromobutanes；
Fig. 4：Two are added during embodiment 1（2- chloroethyls）The Aripiprazole sample gas-chromatography of amine hydrochlorate and 1,4- dibromobutanes
Figure；
Fig. 5：Two are added during embodiment 2（2- chloroethyls）The gas phase color of the Aripiprazole sample of amine hydrochlorate and 1,4- dibromobutanes
Spectrogram；
Fig. 6：Two are added during embodiment 3（2- chloroethyls）The gas phase color of the Aripiprazole sample of amine hydrochlorate and 1,4- dibromobutanes
Spectrogram.
Embodiment：
Following examples are used to further understand the present invention, but are not limited to the scope of this implementation.Below by way of example forms, to this
Invent the relevant substance detecting method of Aripiprazole being related to be described in further detail, but this should not be interpreted as in the present invention
The scope for stating theme is only limitted to following example, and all technologies realized based on the above of the present invention belong to the model of the present invention
Enclose.
Embodiment 1
Instrument and condition
Chromatograph：The plus gas chromatographs of Shimadzu 2010；
Detector：Flame ionization ditector；
Chromatographic column：ZB-50 capillary chromatographic columns（60m × 0.32mm, 0.50 μm）；
Injector temperature：200℃；
Detector temperature：250℃；
Carrier gas（Nitrogen）Flow velocity：3.0ml/min；
Split ratio：2:1；
Sampling volume：1μl.
Column temperature rise program：
。
Experimental procedure
Take Aripiprazole appropriate, plus the solution of the 100mg containing Aripiprazole in every 1ml is made in absolute ethyl alcohol dissolving, is used as A Li piperazines
Azoles sample solution；Take two（2- chloroethyls）Amine hydrochlorate and Isosorbide-5-Nitrae-appropriate dibromobutane, plus absolute ethyl alcohol dissolving are made in every 1ml
Containing two（2- chloroethyls）The solution of amine hydrochlorate and each 5 μ g of Isosorbide-5-Nitrae-dibromobutane, is used as reference substance solution；Separately absolute ethyl alcohol is taken to make
For blank solution.Analyzed by above-mentioned chromatographic condition, chromatogram is recorded, by external standard method with calculated by peak area two（2- chloroethyls）
The content of amine hydrochlorate and 1,4- dibromobutanes.As a result accompanying drawing 1 ~ 4 is seen, Fig. 1 is blank solution chromatogram；Fig. 2 is Aripiprazole
Sample solution chromatogram；Retention time 4.508min chromatographic peak is two in Fig. 3（2- chloroethyls）Amine hydrochlorate, retention time
4.794min chromatographic peak is 1,4- dibromobutanes；Fig. 4 is addition two（2- chloroethyls）Amine hydrochlorate and 1,4- dibromobutanes
Aripiprazole sample gas chromatogram.Fig. 1 ~ Fig. 4 shows：The method that the present invention is provided can fast and effeciently separation determination A Li piperazines
Two in azoles（2- chloroethyls）Amine hydrochlorate and Isosorbide-5-Nitrae-dibromobutane, it is possible to accurately quantitatively detected, so as to reach to A Li
Effective control of piperazine azoles purity and quality.
Embodiment 2
Instrument and condition
Chromatograph：The plus gas chromatographs of Shimadzu 2010；
Detector：Flame ionization ditector；
Chromatographic column：ZB-50 capillary chromatographic columns（60m × 0.32mm, 0.50 μm）；
Injector temperature：205℃；
Detector temperature：250℃；
Carrier gas（Nitrogen）Flow velocity：3.0ml/min；
Split ratio：2:1；
Sampling volume：1μl.
Column temperature rise program：
。
Experimental procedure
Take two（2- chloroethyls）Amine hydrochlorate and Isosorbide-5-Nitrae-appropriate dibromobutane, plus absolute ethyl alcohol dissolving are made in every 1ml and contain two
（2- chloroethyls）The solution of amine hydrochlorate and each 5 μ g of Isosorbide-5-Nitrae-dibromobutane, is used as reference substance solution；Separately absolute ethyl alcohol is taken as sky
White solution.Analyzed by above-mentioned chromatographic condition, record chromatogram.As a result retention time 4.502min in accompanying drawing 5, Fig. 5 is seen
Chromatographic peak is two（2- chloroethyls）Amine hydrochlorate, retention time 4.786min chromatographic peak is Isosorbide-5-Nitrae-dibromobutane.
Embodiment 3
Instrument and condition
Chromatograph：The plus gas chromatographs of Shimadzu 2010；
Detector：Flame ionization ditector；
Chromatographic column：ZB-50 capillary chromatographic columns（60m × 0.32mm, 0.50 μm）；
Injector temperature：200℃；
Detector temperature：250℃；
Carrier gas（Nitrogen）Flow velocity：3.2ml/min；
Split ratio：2:1；
Sampling volume：1μl.
Column temperature rise program：
。
Experimental procedure
Take two（2- chloroethyls）Amine hydrochlorate and Isosorbide-5-Nitrae-appropriate dibromobutane, plus absolute ethyl alcohol dissolving are made in every 1ml and contain two
（2- chloroethyls）The solution of amine hydrochlorate and each 5 μ g of Isosorbide-5-Nitrae-dibromobutane, is used as reference substance solution；Separately absolute ethyl alcohol is taken as sky
White solution.Analyzed by above-mentioned chromatographic condition, record chromatogram.As a result retention time 4.405min in accompanying drawing 6, Fig. 6 is seen
Chromatographic peak is two（2- chloroethyls）Amine hydrochlorate, retention time 4.684min chromatographic peak is Isosorbide-5-Nitrae-dibromobutane.
The present invention is to the relevant material of the Aripiprazole two（2- chloroethyls）Amine hydrochlorate and 1,4- dibromobutanes analysis side
The following items of method are verified：
System suitability is tested
Take Aripiprazole and two（2- chloroethyls）Amine hydrochlorate and Isosorbide-5-Nitrae-appropriate dibromobutane, dissolve sample with absolute ethyl alcohol respectively
Product, are configured to contain Aripiprazole, two（2- chloroethyls）The need testing solution of amine hydrochlorate and 1,4- dibromobutanes.By embodiment 1
Chromatographic condition carry out gas chromatographic analysis, record chromatogram.From Fig. 1 ~ Fig. 4, on this condition two（2- chloroethyls）Amine
Hydrochloride and Isosorbide-5-Nitrae-separating degree is good between dibromobutane and adjacent peak, solvent and Aripiprazole other impurities do not disturb two
（2- chloroethyls）The measure of amine hydrochlorate and Isosorbide-5-Nitrae-dibromobutane, therefore illustrate that the analysis method specificity is good.
Sample introduction replica test
Take the relevant material two of Aripiprazole（2- chloroethyls）Amine hydrochlorate and Isosorbide-5-Nitrae-dibromobutane need testing solution, by embodiment 1
Chromatographic condition, repeat sample introduction 6 times, investigate the repeatability of method.It can be obtained by result, this method sample introduction repeatability is good.
。
Quantitative limit, test limit
Take the relevant material two of Aripiprazole（2- chloroethyls）Amine hydrochlorate and Isosorbide-5-Nitrae-appropriate dibromobutane, it is accurately weighed, respectively
Absolute ethyl alcohol sample dissolution is used, the need testing solution of certain response is configured to, then precision measures need testing solution in right amount, step by step
Dilution, is investigated by the chromatographic condition sample introduction of embodiment 1.Two（2- chloroethyls）Amine hydrochlorate and 1,4- dibromobutanes quantitative limit and inspection
Survey limit data as shown in the table：
。
Linearly
Take the relevant material two of Aripiprazole（2- chloroethyls）Amine hydrochlorate and Isosorbide-5-Nitrae-appropriate dibromobutane, it is accurately weighed, use respectively
Absolute ethyl alcohol dissolves, and is configured to two（2- chloroethyls）Amine hydrochlorate and 1,4- dibromobutane stock solutions；Precision measures two（2- chloroethenes
Base）Amine hydrochlorate and Isosorbide-5-Nitrae-dibromobutane stock solution, be diluted to respectively concentration for 2.5 μ g/ml, 4.0 μ g/ml, 5.0 μ g/ml,
The two of 6.0 μ g/ml and 7.5 μ g/ml（2- chloroethyls）Amine hydrochlorate and Isosorbide-5-Nitrae-dibromobutane need testing solution, by each solution by real
The chromatographic condition sample introduction for applying example 1 is investigated, and as a result see the table below：
。
The degree of accuracy
Take the relevant material two of Aripiprazole（2- chloroethyls）Amine hydrochlorate and Isosorbide-5-Nitrae-appropriate dibromobutane, it is accurately weighed, use respectively
Absolute ethyl alcohol dissolves, and is configured to two（2- chloroethyls）Amine hydrochlorate and 1,4- dibromobutane stock solutions；Precision measures two（2- chloroethenes
Base）Amine hydrochlorate and Isosorbide-5-Nitrae-dibromobutane stock solution are appropriate, are diluted with absolute ethyl alcohol, be made into respectively 4.0 μ g/ml, 5.0 μ g/ml,
6.0 μ g/ml accuracy test solution.Aripiprazole about 100mg is taken, respectively plus the accuracy test solution for stating various concentrations
1mL dissolves, as the need testing solution of various concentrations level, and each concentration level need testing solution is parallel to prepare 3 parts；Separately take A Li
Piperazine azoles about 100mg, adds the dissolving of 1mL absolute ethyl alcohols, is used as blank sample solution.Above-mentioned solution is pressed to the chromatostrip of embodiment 1
Part sample introduction is investigated, and Fig. 4 is 5.0 μ g/ml need testing solutions（Two are added in Aripiprazole（2- chloroethyls）Amine hydrochlorate and 1,4-
Dibromobutane）Chromatogram, the chromatographic peak that retention time is 4.504min is two（2- chloroethyls）Amine hydrochlorate, retention time is
4.788min chromatographic peak is Isosorbide-5-Nitrae-dibromobutane, and sample introduction result see the table below：
。
Durability
By finely tuning the chromatographic conditions such as injector temperature, flow rate of carrier gas, detector temperature and chromatographic column brand, we further examine
The durability of method is examined.As a result find, this method changes ± 5 DEG C, carrier gas stream to the chromatographic columns of different brands, injector temperature
Fast change ± 0.2ml/min, detector temperature change good tolerance under the conditions of ± 5 DEG C of grades.In different brands chromatographic column, difference
Under the conditions of injector temperature, flow rate of carrier gas and detector temperature, two（2- chloroethyls）Amine hydrochlorate and 1,4- dibromobutanes retain
Time can reach and efficiently separate without significant changes.
Claims (7)
1. one kind utilizes the relevant material two of gas chromatography separation detection Aripiprazole（2- chloroethyls）Amine hydrochlorate and 1,4- bis-
The method of NBB, it is characterised in that：From suitable solvent by sample and two（2- chloroethyls）Amine hydrochlorate and 1,4- dibromos
Butane dissolves, according to the formation and physic-chemical property of material to be analyzed, from methyl polysiloxane class chromatographic column and hydrogen flame ion
Change detector.
2. method of separating and assaying according to claim 1, solvent can be sub- for ethanol, methanol, dichloromethane or dimethyl
One or more in sulfone.
3. method of separating and assaying according to claim 1, chromatographic column be selected from brand be Phenomenex, Agilent,
Supelco or Restek chromatographic column.
4. method of separating and assaying according to claim 1, chromatographic column is middle grade or low pole methyl polysiloxane class
Capillary chromatographic column.
5. method of separating and assaying according to claim 1, it is characterised in that including following steps：
1）Take Aripiprazole appropriate, plus the solution of the 100mg containing Aripiprazole in every 1ml is made in absolute ethyl alcohol dissolving, as trying
Product solution；Separately take two（2- chloroethyls）Amine hydrochlorate and Isosorbide-5-Nitrae-appropriate dibromobutane, plus absolute ethyl alcohol dissolving are made in every 1ml and contained
Two（2- chloroethyls）The solution of amine hydrochlorate and each 5 μ g of Isosorbide-5-Nitrae-dibromobutane, is used as reference substance solution；
2）It is 200 ~ 250 DEG C to set injector temperature, and flow rate of carrier gas is 1.0 ~ 3.5ml/min, programmed temperature method, and heating schedule is
135 °C of initial temperature, 1 ~ 3min of constant temperature, with 8 ~ 15 °C per minute of heating rate to 160 °C, 2 ~ 5min of constant temperature, detector temperature
Spend for 250 ~ 300 DEG C, split ratio is 2:1~10:1；
3）Take 1）Middle need testing solution and each 1~3 μ l of reference substance solution, by 2）Chromatographic condition, inject gas chromatograph, use
External standard method is calculated two in Aripiprazole（2- chloroethyls）The content of amine hydrochlorate and 1,4- dibromobutanes.
6. method for separating and analyzing according to claim 5, step 2）Described carrier gas is nitrogen or helium.
7. method for separating and analyzing according to claim 5, step 2）Described programmed temperature method, preferably following heating journey
Sequence：
。
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110836930A (en) * | 2018-08-17 | 2020-02-25 | 万特制药(海南)有限公司 | Method for measuring content of dichlorobutane in levetiracetam by gas chromatography-mass spectrometry |
| CN111551652A (en) * | 2020-06-28 | 2020-08-18 | 珠海润都制药股份有限公司 | Method for detecting bromobutane in irbesartan |
| CN112114080A (en) * | 2019-06-20 | 2020-12-22 | 扬子江药业集团南京海陵药业有限公司 | Method for detecting aripiprazole related substances |
| CN112114051A (en) * | 2019-06-20 | 2020-12-22 | 扬子江药业集团南京海陵药业有限公司 | Method for detecting genotoxic impurity halogenated alkane in aripiprazole |
| CN113514564A (en) * | 2020-04-10 | 2021-10-19 | 昆药集团股份有限公司 | Method for detecting residues 1, 2-dibromoethane and 1, 3-dibromopropane in homopiperazine |
| CN115436528A (en) * | 2022-10-08 | 2022-12-06 | 常州佳德医药科技有限公司 | Method for detecting purity of 2, 6-dimethylpiperazine by gas chromatography |
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| CN106501387A (en) * | 2016-09-21 | 2017-03-15 | 北京万全德众医药生物技术有限公司 | A kind of method of use gas chromatography separation determination aripiprazole intermediate about material |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110836930A (en) * | 2018-08-17 | 2020-02-25 | 万特制药(海南)有限公司 | Method for measuring content of dichlorobutane in levetiracetam by gas chromatography-mass spectrometry |
| CN112114080A (en) * | 2019-06-20 | 2020-12-22 | 扬子江药业集团南京海陵药业有限公司 | Method for detecting aripiprazole related substances |
| CN112114051A (en) * | 2019-06-20 | 2020-12-22 | 扬子江药业集团南京海陵药业有限公司 | Method for detecting genotoxic impurity halogenated alkane in aripiprazole |
| CN112114080B (en) * | 2019-06-20 | 2022-05-13 | 扬子江药业集团南京海陵药业有限公司 | Method for detecting aripiprazole related substances |
| CN113514564A (en) * | 2020-04-10 | 2021-10-19 | 昆药集团股份有限公司 | Method for detecting residues 1, 2-dibromoethane and 1, 3-dibromopropane in homopiperazine |
| CN111551652A (en) * | 2020-06-28 | 2020-08-18 | 珠海润都制药股份有限公司 | Method for detecting bromobutane in irbesartan |
| CN115436528A (en) * | 2022-10-08 | 2022-12-06 | 常州佳德医药科技有限公司 | Method for detecting purity of 2, 6-dimethylpiperazine by gas chromatography |
| CN115436528B (en) * | 2022-10-08 | 2024-03-19 | 常州佳德医药科技有限公司 | Method for detecting purity of 2, 6-dimethylpiperazine by adopting gas chromatography |
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Application publication date: 20170915 |