Distinguishing and determining method of entecavir chiral isomers
What is Al technical title?
Al technical title is built by PatSnap Al team. It summarizes the technical point description of the patent document.
A technology for chiral isomers and entecavir, applied in the field of mass spectrometry analysis, can solve the problems of insufficient enantiomeric separation, long solvent gradient elution time, no simultaneous separation of chiral isomers, etc., so as to improve the separation efficiency. , method fast effect
Active Publication Date: 2018-03-06
HANGZHOU LEADING PHARMATECH CO LTD +1
View PDF3 Cites 8 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
At present, the existing methods for separating entecavir chiral isomers are mainly high-performance liquid chromatography. These methods require specific chiral stationary phases, and the solvent gradient elution takes a long time, and cannot realize the eight chiral isomers of entecavir. The separation ...
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.
Smart Image
Examples
Experimental program
Comparison scheme
Effect test
Embodiment 1
[0030] 1) Analytical sample preparation: the pure products of each single configuration of entecavir are dissolved in 50v / v% methanol aqueous solution to prepare 100μg / ml standard solution for use, and R-besifloxacin powder is dissolved in methanol to 1mg / ml For use, metal salt ZnSO 4 The powder was dissolved and diluted in ultrapure water into a 1mg / ml stock solution for later use; the standard solutions of each configuration of entecavir were used with R-besifloxacin solution and ZnSO respectively 4 Solution mixing; final concentration of entecavir in each mixed solution is 25μg / ml, final concentration of R-besifloxacin is 25μg / ml, ZnSO 4 The final concentration is 2.5μg / ml.
[0031] 2) Determine the working conditions of the mass spectrometer: Bruker ion trap mass spectrometer is used, the electrospray ion source is selected, and the data is processed by Compass DataAnalysis software. Instrument parameter settings: spray needle voltage, -4500V; nitrogen as atomizing gas, pressu...
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
Login to view more
Abstract
The invention discloses a distinguishing and determining method of entecavir chiral isomers. The method comprises the steps of adopting a chiral ligand, metal ions and the eight entecavir chiral isomers to form complexes with different stable forms; utilizing a mass-spectrography method for recognizing and distinguishing the complexes, wherein the chiral ligand comprises R-besifloxacin, beta-cyclodextrin, migltol or cefotaxime; the metal ions comprise alkaline-earth metals or transient state metals; the alkaline-earth metals comprise Mg and Ca; the transient state metals comprise Ni, Cu, Co, Zn and Mn. The method is fast, simple and convenient, overcomes the defects that a traditional HPLC method needs a specific chiral stationary phase, solvent gradient eluting consumed time is longer, and an enantiomeric separation degree is insufficient, and can be used for quickly distinguishing the eight entecavir chiral isomers and quantitatively determining.
Description
Technical field [0001] The invention belongs to the technical field of mass spectrometry, and is used for distinguishing chiral isomers of medicines, in particular to a mass spectrometry kinetic method for separating entecavir chiral isomers. Background technique [0002] Entecavir (entecavir, ETV) is a cyclopentylguanosine nucleoside analogue. At present, this drug is the first-line drug for the antiviral treatment of chronic hepatitis B. There are 3 chiral centers in its structure, which can produce 8 optical anomalies. Conform, clinical medication is a single isomer (1S, 3R, 4S). (1S, 3R, 4S); (1R, 3S, 4R); (1S, 3S, 4R); (1R, 3R, 4S); (1S, 3R, 4R); (1R, 3S, 4S); ( 1R, 3R, 4R); (1S, 3S, 4S) These 8 configurations correspond to the numbers ETV1; ETV2; ETV3; ETV4; ETV5; ETV6; ETV7; ETV8. The structural formula of ETV1 is as follows: [0003] [0004] According to the relevant provisions of the guidelines for the analysis of drug impurities in the 2015 Chinese Pharmacopoeia, in a...
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.
Login to view more 
Login to view more