A kind of hplc detection method of pitavastatin isopropyl tert-butyl ester diastereomer

A technology of diastereoisomers and propyl tert-butyl ester, which is applied in the field of drug detection and can solve problems affecting the detection of the content of pitavastatin isopropyl tert-butyl ester

Active Publication Date: 2022-07-12
SHIJIAZHUANG NO 4 PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Because the existence of above two kinds of diastereoisomers can affect the detection of pitavastatin isopropyl tert-butyl ester content, and there is no effective separation and detection of pitavastatin isopropyl tert-butyl ester at present. Therefore, there is an urgent need for a fast and accurate method for the separation and detection of diastereomers of pitavastatin isopropyl tert-butyl ester

Method used

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  • A kind of hplc detection method of pitavastatin isopropyl tert-butyl ester diastereomer
  • A kind of hplc detection method of pitavastatin isopropyl tert-butyl ester diastereomer
  • A kind of hplc detection method of pitavastatin isopropyl tert-butyl ester diastereomer

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 1. Instruments and Conditions

[0037] Chromatographic column: amylose-tris(tri-chloro-penta-methylphenylcarbamate) as filler, size: 4.6mm×250mm, 3μm;

[0038] Mobile phase: water-acetonitrile with a volume ratio of 35:65;

[0039] Column temperature: 30℃;

[0040] Detection wavelength: 245nm;

[0041] Flow rate: 0.5mL / min;

[0042] Elution method: isocratic elution;

[0043] Diluent: water and acetonitrile are evenly mixed in a volume ratio of 2:3 to obtain a diluent;

[0044] Test solution: take 10 mg of pitavastatin isopropyl tert-butyl ester test product, accurately weigh it, place it in a 100mL volumetric flask, and dilute it to the mark with diluent as the test solution;

[0045] Take (4R-6R)-6-[[(1E)-2-cyclopropyl-4-(4-fluorophenyl)-3-quinolinyl]vinyl]-2,2-dimethyl-1 , 3-dioxane-4-acetic acid tert-butyl ester (diastereomer A) reference substance, diluted with diluent gradient to 0.5μg / mL, to obtain reference substance solution A;

[0046] Take (4S-6S)-6-[[...

Embodiment 2

[0050] 1. Instruments and Conditions

[0051] Chromatographic column: amylose-tris(tri-chloro-penta-methylphenylcarbamate) as filler, size: 4.6mm×250mm, 3μm;

[0052]Mobile phase: water-acetonitrile with a volume ratio of 35:60;

[0053] Column temperature: 28℃;

[0054] Detection wavelength: 243nm;

[0055] Flow rate: 0.2mL / min;

[0056] Elution method: isocratic elution;

[0057] Diluent: water and acetonitrile are evenly mixed in a volume ratio of 2:2.5 to obtain a diluent;

[0058] Test solution: take 8 mg of pitavastatin isopropyl tert-butyl ester test product, accurately weigh it, place it in a 100mL volumetric flask, and dilute it to the mark with diluent as the test solution;

[0059] Take diastereomer A(4R-6R)-6-[[(1E)-2-cyclopropyl-4-(4-fluorophenyl)-3-quinolinyl]vinyl]-2, 2-Dimethyl-1,3-dioxane-4-acetic acid tert-butyl ester reference substance, diluted with diluent gradient to 0.4μg / mL, to obtain reference substance solution A;

[0060] Take diastereomer B(4...

Embodiment 3

[0064] 1. Instruments and Conditions

[0065] Chromatographic column: amylose-tris(tri-chloro-penta-methylphenylcarbamate) as filler, size: 4.6mm×250mm, 3μm;

[0066] Mobile phase: water-acetonitrile with a volume ratio of 35:70;

[0067] Column temperature: 32℃;

[0068] Detection wavelength: 247nm;

[0069] Flow rate: 1mL / min;

[0070] Elution method: isocratic elution;

[0071] Diluent: water and acetonitrile are evenly mixed in a volume ratio of 2:3.5 to obtain a diluent;

[0072] Test solution: take 12 mg of pitavastatin isopropyl tert-butyl ester test product, accurately weigh it, place it in a 100mL volumetric flask, dilute it to the mark with diluent, and use it as the test solution;

[0073] Take diastereomer A(4R-6R)-6-[[(1E)-2-cyclopropyl-4-(4-fluorophenyl)-3-quinolinyl]vinyl]-2, 2-Dimethyl-1,3-dioxane-4-acetic acid tert-butyl ester reference substance, diluted with diluent gradient to 0.6μg / mL, to obtain reference substance solution A;

[0074] Take diastere...

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Abstract

The invention relates to the technical field of drug detection, and specifically discloses an HPLC detection method for diastereomers of pitavastatin isopropyl tert-butyl ester. The chromatographic conditions of the HPLC detection method of the diastereomer of pitavastatin isopropyl tert-butyl ester are: chromatographic column: amylose-tris(3-chloro-5-methylphenylcarbamate) is a filler; mobile phase: water and acetonitrile with a volume ratio of 35:60‑70; column temperature: 28‑32℃; detection wavelength: 243‑247nm; flow rate: 0.2‑1mL / min; elution method: isocratic wash take off. The HPLC detection method for diastereomer of pitavastatin isopropyl tert-butyl ester provided by the invention can realize the simultaneous detection of two diastereomers in pitavastatin isopropyl tert-butyl ester, and the precise High accuracy, high reproducibility and good reproducibility provide a reliable guarantee for improving and controlling the quality of pitavastatin isopropyl tert-butyl ester and the final product pitavastatin calcium.

Description

technical field [0001] The invention relates to the technical field of drug detection, in particular to an HPLC detection method for diastereomers of pitavastatin isopropyl tert-butyl ester. Background technique [0002] Pitavastatin isopropyl tert-butyl ester is an intermediate for the synthesis of pitavastatin calcium. The Chinese name of pitavastatin isopropyl tert-butyl ester is: (4R-6S)-6-[[(1E)-2-ring Propyl-4-(4-fluorophenyl)-3-quinolinyl]vinyl]-2,2-dimethyl-1,3-dioxane-4-acetic acid tert-butyl ester, its English name as: (4R,6S)-6-[(1E)-2-[2-Cyclopropyl-4-(4-fluorophenyl)-3-quinolinyl]ethenyl]-2,2-dimethyl-1,3-dioxane-4 -acetic acidtert-butyl ester, molecular formula: C 32 H 36 FNO 4 , and its structural formula is: [0003] [0004] (4R-6S)-6-[[(1E)-2-cyclopropyl-4-(4-fluorophenyl)-3-quinolinyl]vinyl]-2,2-dimethyl-1, 3-Dioxane-4-acetic acid tert-butyl ester exists in two diastereomers, which are (4R-6R)-6-[[(1E)-2-cyclopropyl-4-(4- Fluorophenyl)-3-quinolin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/89
CPCG01N30/89
Inventor 张煜玲杨俊免李彪刘清萍焦立苗陈伟贾萧铭马明卓
Owner SHIJIAZHUANG NO 4 PHARMA
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