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HPLC detection method for statins starting material and enantiomer thereof

A technology of enantiomers and detection methods, which is applied in the field of HPLC detection of statin drug starting materials and their enantiomers, can solve complex operation steps, unsatisfactory accuracy and sensitivity, and low detection efficiency problem, to achieve the effect of improving detection efficiency, improving and controlling quality, high accuracy and sensitivity

Active Publication Date: 2021-06-11
SHIJIAZHUANG NO 4 PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Due to the presence of (4S-cis)-6-formyl-2,2-dimethyl-1,3-dioxane-4-acetic acid tert-butyl ester can affect the detection of statin drug starting material content, and At present, there is no effective method for separating and detecting the enantiomers of the starting materials of statins, and the current method for detecting the enantiomers of the starting materials of statins needs to control many factors, and the operation steps Complicated, low detection efficiency, poor accuracy and sensitivity

Method used

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  • HPLC detection method for statins starting material and enantiomer thereof
  • HPLC detection method for statins starting material and enantiomer thereof
  • HPLC detection method for statins starting material and enantiomer thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0035] 1. Instrument and conditions Chromatographic column: chiral chromatographic column with cellulose-tris(4-methylbenzoate) coated silica gel as filler; specification: 150mm×4.6mm, 5μm;

[0036] Mobile phase: sodium acetate buffer and acetonitrile with a volume ratio of 68:32; wherein, the sodium acetate buffer is 0.151 mg / mL sodium acetate aqueous solution plus glacial acetic acid to adjust the pH to 5.0;

[0037] Column temperature: 30°C;

[0038] Detection wavelength: 242nm;

[0039] Injection volume: 10μL;

[0040] Flow rate: 0.5mL / min;

[0041] Elution method: isocratic elution;

[0042] Solvent: water and acetonitrile are obtained by mixing uniformly at a volume ratio of 1:1;

[0043] Derivatization reagent: adding salicylic hydrazide to the solvent to obtain a reagent with a salicylic hydrazide concentration of 1 mg / mL;

[0044] Need testing solution: get the test sample of the statin drug starting material, add solvent and ultrasonically dissolve to make a sol...

Embodiment 2

[0093] 1. Instrument and conditions Chromatographic column: chiral chromatographic column with cellulose-tris(4-methylbenzoate) coated silica gel as filler; specification: 150mm×4.6mm, 5μm;

[0094] Mobile phase: sodium acetate buffer and acetonitrile with a volume ratio of 65:32; wherein, the sodium acetate buffer is 0.148 mg / mL sodium acetate aqueous solution plus glacial acetic acid to adjust the pH to 4.5;

[0095] Column temperature: 28°C;

[0096] Detection wavelength: 240nm;

[0097] Injection volume: 8μL;

[0098] Flow rate: 0.4mL / min;

[0099] Elution method: isocratic elution;

[0100] Solvent: water and acetonitrile are obtained by mixing uniformly at a volume ratio of 1:0.8;

[0101] Derivatization reagent: adding salicylhydrazide to the solvent to obtain a reagent with a concentration of salicylhydrazide of 0.8 mg / mL;

[0102] Need test solution: take the test sample of the statin drug starting material, add solvent and ultrasonically dissolve to make a solut...

Embodiment 3

[0109] 1. Instrument and conditions Chromatographic column: chiral chromatographic column with cellulose-tris(4-methylbenzoate) coated silica gel as filler; specification: 150mm×4.6mm, 5μm;

[0110] Mobile phase: sodium acetate buffer and acetonitrile with a volume ratio of 70:32; wherein, the sodium acetate buffer is 0.153 mg / mL sodium acetate aqueous solution plus glacial acetic acid to adjust the pH to 5.5;

[0111] Column temperature: 32°C;

[0112] Detection wavelength: 244nm;

[0113] Injection volume: 12μL;

[0114] Flow rate: 0.6mL / min;

[0115] Elution method: isocratic elution;

[0116] Solvent: water and acetonitrile are obtained by mixing uniformly at a volume ratio of 1:1.2;

[0117] Derivatization reagent: adding salicylhydrazide to the solvent to obtain a reagent with a concentration of salicylhydrazide of 1.2 mg / mL;

[0118] Need test solution: take the test sample of the statin drug starting material, add solvent and ultrasonically dissolve to make a solu...

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Abstract

The invention relates to the technical field of medicine detection, and particularly discloses an HPLC detection method for a statins starting material and enantiomer thereof. According to chromatographic conditions of the HPLC detection method for the statins starting material and the enantiomer, a chromatographic column is a chiral chromatographic column taking cellulose-tri (4-methyl benzoate) coated silica gel as a filler; a mobile phase comprises a sodium acetate buffer solution and acetonitrile in a volume ratio of (65-70): 32; the column temperature is 28-32 DEG C; the detection wavelength is 240 to 244nm; and the elution mode is isocratic elution. The HPLC detection method for the statins starting material and the enantiomer thereof provided by the invention can meet accurate detection of the enantiomer of the statins starting material, is high in precision, accuracy and sensitivity and high in reproducibility and stability, and can be used for quality control and comprehensive evaluation of the statins starting material.

Description

technical field [0001] The invention relates to the technical field of drug detection, in particular to an HPLC detection method for statin drug starting materials and their enantiomers. Background technique [0002] The Chinese name of the starting material of statins is: (4R-cis)-6-formaldehyde-2,2-dimethyl-1,3-dioxane-4-tert-butyl acetate, and its English name is : tert-butyl(4R-cis)-6-formaldehyde-2,2-dimethyl-1,3-dioxane-4-acetate, molecular formula: C 13 h 22 o 5 , whose structural formula is: [0003] [0004] The enantiomer of (4R-cis)-6-formyl-2,2-dimethyl-1,3-dioxane-4-acetic acid tert-butyl ester is: (4S-cis)-6- Aldehyde-2,2-dimethyl-1,3-dioxane-4-acetic acid tert-butyl ester, its structural formula is: [0005] [0006] Due to the presence of (4S-cis)-6-formyl-2,2-dimethyl-1,3-dioxane-4-acetic acid tert-butyl ester can affect the detection of statin drug starting material content, and At present, there is no effective method for separating and detecti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/884
Inventor 张煜玲杨俊免李彪刘清萍温雅闫菲马明卓王晓霞王肖
Owner SHIJIAZHUANG NO 4 PHARMA
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