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Detection method of propofol fumarate tenofovir isomer

A technology of propofol fumarate and tenofovir, which is applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of single detection structure and inability to meet the requirements of baseline separation.

Pending Publication Date: 2021-07-06
REYOUNG PHARMA
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Problems solved by technology

[0004] Patent CN01813161.1 Nucleotide phosphate analog prodrug and its screening and preparation method discloses an analysis method for the separation and detection of diastereoisomers of tenofovir alafenamide fumarate using reverse-phase HPLC , the detection structure is single
[0005] Patent CN111189947A discloses an analytical method for separating and detecting tenofovir alafenamide isomers, using Daicel bonded chiral chromatography column CHIRALPAK IC column, mobile phase is n-hexane, isopropanol, methanol, ethanol, A mixed solution of one or more of methyl tert-butyl ether, tetrahydrofuran, dichloromethane, chloroform, ethyl acetate and acetonitrile, the additive is diethylamine or ethylenediamine, and the separation of isomer impurities is Diastereomer SSS, Diastereomer RSR, Enantiomer SRR, Phosphorus Isomer RRS, Diastereomer RRR, Diastereomer SRS, Diastereomer Body SSR, its embodiment 2 and attached Figure 5 It shows that the combination and proportion of the mobile phase and the selection of the column cannot meet the requirements of the baseline separation in the method detection

Method used

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  • Detection method of propofol fumarate tenofovir isomer
  • Detection method of propofol fumarate tenofovir isomer
  • Detection method of propofol fumarate tenofovir isomer

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0084] Establishment and condition optimization of detection methods:

[0085] Limit specification:

[0086] Isomeric impurities, according to general impurities, according to human drug registration technology International Coordination Conference (ICH) guidelines, limited to 0.10%, as a reference foundation for detection method development.

[0087] Each isomer impurity has a maximum absorption wavelength at around 260 nm, and the detection wavelength can be selected from 258 nm to 262 nm. The present embodiment is preferably 260 nm; when the amount of intake is 20 μl, each isomer impurity peak is a minimum of 0.5mV, It has been able to meet the sensitivity requirements of the method, so it is determined that the concentration of the tester is 0.5 mg / ml, the isomer gas concentration is 0.5 μg / ml, and each isomer impurity is formulated according to the concentration of the test. And impurities positioning solutions.

[0088] Screening of columns:

[0089] The concentration of...

Embodiment 2

[0112] Verify system applicability and exclusive

[0113] Solution preparation:

[0114] Blank solvent: absolute ethanol, diluent;

[0115] Isomeric stocks: 10 mg of TAF-6-A, TAF-6-A1 and TAF-6-A3, respectively, and are precisely determined, respectively, respectively, respectively, 20 ml of four different 20 ml, respectively. In the volumetric flask, the dilute agent is dissolved and diluted to the scale to obtain isomer reserve, wherein TAF-6-A, TAF (free state), TAF-6-A1 peak 1, TAF-6-A1 peak 2, TAF- 6-A3 peaks 1, TAF-6-A3 peak 2 and TAF-6-A2 peak concentrations are about 0.5 mg / ml, respectively;

[0116] Systematic Solution: Add 5 mg of the propylene glycassolidinolifuli raw material medicine to 20 mg, precisely 20mL volumetric flask, add 0.2ml of the isomer reserve, dissolve and dilute to the scale, Get systematic applicability solution, where fumarate propanol replacement Novir concentration is about 0.5 mg / ml, TAF-6-A, TAF-6-A1 peak 1, TAF-6-A1 peak 2, TAF-6- A3 peaks 1...

Embodiment 3

[0127] Verify detection limit and quantitative limit:

[0128] Solution preparation:

[0129] Blank solvent: absolute ethanol, diluent;

[0130] Isomeric stocks: 10 mg of TAF-6-A, TAF-6-A1 and TAF-6-A3, respectively, and are precisely determined, respectively, respectively, respectively, 20 ml of four different 20 ml, respectively. In the volumetric flask, the dilute agent is dissolved and diluted to the scale to obtain isomer reserve, wherein TAF-6-A, TAF (free state), TAF-6-A1 peak 1, TAF-6-A1 peak 2, TAF- 6-A3 peaks 1, TAF-6-A3 peak 2 and TAF-6-A2 peak concentrations are about 0.5 mg / ml, respectively;

[0131] Isomeric positioning solution: 1 ml of each of the numeral reserve is used to separate four different 50 mL of volumetric flask, diluted to the scale, shake well with a diluent, to obtain an isomer-locating solution, wherein TAF-6-A, Taf (free state), TAF-6-A1 peak 1, TAF-6-A1 peak 2, TAF-6-A3 peak 1, TAF-6-A3 peak 2 and TAF-6-A2 peak concentrations are about 10 μg / ml...

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Abstract

The invention relates to the technical field of drug analysis and detection, and particularly relates to a detection method of a propofol fumarate tenofovir isomer. The detection method of the propofol fumarate tenofovir isomer comprises a chromatographic column: a chiral chromatographic column; mobile phases: normal hexane, absolute ethyl alcohol, methanol and diethylamine; a detection wavelength: 260 nm; a column temperature: 30 DEG C; a flow rate: 1.0 ml / min; preparation of a solution; and high performance liquid chromatography detection. The chiral chromatographic column is a normal-phase chromatographic column taking a derivative of amylose as a stationary phase; and the volume ratio of the normal hexane to the absolute ethyl alcohol to the methanol in the mobile phase is 65: 25: 10, and the volume of the diethylamine is 0.1% of the total volume sum of the normal hexane, the absolute ethyl alcohol and the methanol. The invention provides the detection method of the propofol fumarate tenofovir isomer, which has the advantages of effective separation of isomer impurities, high sensitivity, good specificity and accurate evaluation of a isomer content of a bulk drug, and has very important significance for clinical medication safety.

Description

Technical field [0001] The present invention relates to the field of drug analysis detection, and more particularly to detecting methods of fumarate propylene phenolifuli isomers. Background technique [0002] Isomers are compounds which are different and structural formulas. Although the chemical composition of isomers is the same, the atoms are different in the space arrangement, which makes their physics, chemical properties or toxicity. Both the pharmaceutical development process involves the study of its isomer impurities. The isomer is substantially different from which is only the difference between the spatial structure, so it is difficult to meet the requirements in conventional inverting high performance liquid chromatography (RP-HPLC) and common columns, generally in RP-HPLC. The retaining time is coincident or the separation is less than 1.5. It is common to use a positive chromatography to study the chromatographic column to study it, which is greater than 1.5, which...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/36G01N30/74G01N30/86
CPCG01N30/02G01N30/06G01N30/34G01N30/36G01N30/74G01N30/8679
Inventor 辛秀民李广高峰孔霁虹李具伟孙永丽王辉甘兴杰
Owner REYOUNG PHARMA
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