Method for detecting brexpiprazole related substance
Active Publication Date: 2020-11-10
四川弘远药业有限公司
View PDF7 Cites 4 Cited by
Summary
Abstract
Description
Claims
Application Information
AI Technical Summary
This helps you quickly interpret patents by identifying the three key elements:
Problems solved by technology
Method used
Benefits of technology
Problems solved by technology
CN105399736A uses octadecylsilane bonded silica gel as a chromatographic column, mobile phase A is sodium octane sulfonate solution, mobile phase B is acetonitrile, detection wavelength is 290nm, flow rate is 1.0ml / min for linear gradient elution, The quinoline dimer can be detected, but the inventor repeated the method in the application to detect ebiprazole and its 6 related substances, only 5 impurities could be detected, and the peaks of the related substances overlapped with the peaks of the drug, This method cannot effectively separate ebiprazole and its related substances
CN107525877A discloses a chromatographic column with octadecylsilane bonded silica gel as filler, phosphate buffer as mobile phase A, mixed solvent of methanol and acetonitrile as mobile phase B, detection wavelength of 225nm, and flow rate of 1.0ml / min, using the gradient elution method to detect ebiprazole and its 6 related substances, but the inventor repeated the application conditions to detect ebiprazole and its 6 related substances, and the separation of related substances could not meet the methodological requirements
Method used
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more
Image
Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
Click on the blue label to locate the original text in one second.
Reading with bidirectional positioning of images and text.
[0112] Mobile phase: mobile phase A: 0.1% formic acid-acetonitrile solution, mobile phase B: 0.1% formic acid-0.04mol / L ammonium chloride solution
[0113] Flow rate: 1.0ml / min
[0114] Column temperature: 35°C
[0115] Detection wavelength: 254nm
[0116] Carry out gradient elution according to the table below:
[0117]
[0118] 2. Operation steps
[0119] Accurately weigh appropriate amounts of ebiprazole reference substance and impurity BPZ-8, BPZ-9, BPZ-16, BPZ-23, BPZ-20, BPZ-29 reference substance, and diluent [0.02mol / LNa 2 SO 4 -acetonitrile-methanol-glacial acetic acid (56:33:11:1)] was dissolved and quantitatively diluted to make a mixed solution containing about 0.4 mg of ebiprazole and 0.8 μg of BPZ impurity per 1 ml as a system suitability solution. Inject 20 μl into the liquid chromatogra...
Embodiment 2
[0124] Example 2 Ebiprazole bulk drug accelerated test (40°C ± 2°C temperature, 75% ± 5% relative humidity) sample detection
[0127] Mobile phase: mobile phase A: acetonitrile solution, mobile phase B: 0.04mol / L ammonium chloride solution
[0128] Wavelength: 254nm;
[0129] Flow rate: 1.0ml / min;
[0130] Column temperature: 35°C;
[0131] Injection volume: 20ul;
[0132] The elution gradient is shown in the table below:
[0133]
[0134] 2. Operation method: Accurately weigh about 10 mg of ebiprazole crude drug after the accelerated test, put it in a 25ml measuring bottle, add an appropriate amount of diluent and shake to dissolve, dilute to the mark with diluent to obtain the test solution. Precision measures need testing solution 0.5ml, puts in 100ml measuring bottle, with diluent [0.02mol / LNa 2 SO 4 -acetonitrile-methanol-glacial acetic acid (56:33:11:...
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more
PUM
Property
Measurement
Unit
wavelength
aaaaa
aaaaa
wavelength
aaaaa
aaaaa
Login to view more
Abstract
The invention provides a method for detecting a brexpiprazole related substance, and the method adopts a chromatographic column with octadecylsilane chemically bonded silica as a filler, an acetonitrile solution as a mobile phase A and an ammonium chloride solution as a mobile phase B, and adopts gradient elution to determine brexpiprazole and related substances thereof. According to the method, brexpiprazole can be effectively separated from adjacent impurities and various impurities, the separation degree is high, brexpiprazole and related substances thereof can be accurately detected, the problem that brexpiprazole and related substances thereof are difficult to separate and detect is effectively solved, and therefore it is guaranteed that the quality of brexpiprazole is controllable.
Description
technical field [0001] The invention relates to a method for detecting related substances of ebiprazole, which belongs to the field of pharmaceutical analytical chemistry. Background technique [0002] Brexpiprazole (Brexpiprazole) is a dopamine, partial 5-HT1A receptor agonist and 5-HT2A receptor antagonist compound used for the treatment of severe depression and schizophrenia. The chemical name of ebiprazole is 7-(4-(4benzo[b]thiophen-4-ylpiperazin-1-yl)butoxy-1H-quinolin-2-one, molecular formula: C 25 h 27 N 3 o 2 S, molecular weight: 433.57, its chemical structural formula is: [0003] [0004] In the process of compound synthesis, important intermediates and impurities may affect the purity and quality of the drug due to incomplete removal. These known intermediates and impurities and the resulting degradation products are related substances. The research on related substances is one of the key items in drug quality research, which affects the stability and safe...
Claims
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more
Application Information
Patent Timeline
Application Date:The date an application was filed.
Publication Date:The date a patent or application was officially published.
First Publication Date:The earliest publication date of a patent with the same application number.
Issue Date:Publication date of the patent grant document.
PCT Entry Date:The Entry date of PCT National Phase.
Estimated Expiry Date:The statutory expiry date of a patent right according to the Patent Law, and it is the longest term of protection that the patent right can achieve without the termination of the patent right due to other reasons(Term extension factor has been taken into account ).
Invalid Date:Actual expiry date is based on effective date or publication date of legal transaction data of invalid patent.