Application of solid-phase extraction column in analysis of tacrolimus preparation impurities

A technology of solid phase extraction column and tacrolimus, which is applied in the application field of solid phase extraction column in the analysis of impurities in tacrolimus ointment, can solve the problems of separation of tacrolimus and its related substances, and achieves safety Effective control of sex and precise control of impurities

Inactive Publication Date: 2019-05-31
GUANGZHOU MEDCAN PHARMATECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The matrix composition of tacrolimus ointment is mainly composed of complex mixtures such as paraffin, liquid paraffin, white petrolatum, and beeswax. Conventional solvent extraction or extraction methods cannot effectively separate tacrolimus and its related substances. Control is a very important link in the field of drug research and development, which is directly related to the stability, effectiveness and safety of the drug. Therefore, it is particularly important to develop an effective tacrolimus ointment sample processing method to control the quality of the drug

Method used

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  • Application of solid-phase extraction column in analysis of tacrolimus preparation impurities
  • Application of solid-phase extraction column in analysis of tacrolimus preparation impurities
  • Application of solid-phase extraction column in analysis of tacrolimus preparation impurities

Examples

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Embodiment 1

[0039] A kind of application of solid phase extraction column in tacrolimus preparation impurity analysis, comprises the following steps:

[0040]a) Rinse the centrifuge tube and the pear-shaped bottle twice with methanol, 5ml each time, and dry them for later use; b) Weigh about 1.0g of tacrolimus blank preparation and tacrolimus preparation samples, 7 samples each, and set In a stoppered glass centrifuge tube; c) Add 5ml of n-hexane-ethyl acetate (10:1) mixed solution to the centrifuge tube respectively, shake vigorously until the suspension is complete; d) Centrifuge at a speed of 3000 rpm for 5 minutes , the supernatant is used as the liquid to be purified; e) the glycol-based silane bonded silica gel solid-phase extraction column is Agilent BondElute 2OH 6cc / 500mg, Waters Sep-Pak 6cc / 500mg, Simon Aldrich Classic 6cc / 500mg, Welchrom 6cc / 500mg , CNWBOND 6cc / 500mg, Merck 6cc / 500mg, Supelco 6cc / 500mg two each, rinse with 5ml of acetonitrile respectively, then rinse twice with...

Embodiment 2

[0044] A kind of application of solid phase extraction column in tacrolimus preparation impurity analysis, comprises the following steps:

[0045] a) Rinse the centrifuge tube and pear-shaped bottle twice with methanol, 5ml each time, and dry for later use; b) Weigh about 1.0 g of tacrolimus blank preparation, 8 parts, and put them in glass centrifuge tubes with stoppers; c ) respectively add 1ml of the mixed reference substance solution to the centrifuge tube, then add 4ml of the mixed solution of n-hexane-ethyl acetate (10:1), shake vigorously until the suspension is complete; d) Centrifuge at a speed of 3000 rpm for 5 minutes , the supernatant is used as the liquid to be purified; e) Take glycol-based silane-bonded silica gel SPE columns Agilent BondElute 2OH 6cc / 500mg, Waters Sep-Pak 6cc / 500mg, Simon Aldrich Classic 6cc / 500mg, Welchrom 6cc / 500mg, CNWBOND 6cc / 500mg, Merck6cc / 500mg, Supelco 6cc / 500mg two each, rinse with 5ml of acetonitrile respectively, then rinse twice wit...

Embodiment 3

[0051] A kind of application of solid phase extraction column in tacrolimus preparation impurity analysis, comprises the following steps:

[0052] a) Rinse the centrifuge tube and the pear-shaped bottle twice with methanol, 5ml each time, and dry it for later use; b) Weigh about 0.5g of tacrolimus blank preparation, 6 parts, and put them in glass centrifuge tubes with stoppers; c ) into 4 centrifuge tubes, add 0.5ml of the mixed reference substance solution, then add 2.5ml of the mixed solution of n-hexane-ethyl acetate (10:1), add n-hexane-ethyl acetate to the other 2 centrifuge tubes respectively (10:1) mixed solution 3ml, shake vigorously until the suspension is complete; d) centrifuge at a speed of 3000 rpm for 5 minutes, and the supernatant is used as the liquid to be purified; e) take a glycol silane bonded silica gel solid phase Extraction column Waters Sep-Pak Diol different specification 1cc / 100mg, 3cc / 200mg each 3 pieces, rinse with 3ml of acetonitrile respectively, ...

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Abstract

The invention relates to an application of a solid-phase extraction column in analysis of tacrolimus preparation ointment. In the preparation process of the test sample, the solid-phase extraction column with diol silane bonded silica gel as a filler is adopted for purification, and through the steps of suspension, activating, sample loading, leaching and elution, the tacrolimus and related substances thereof in the tacrolimus ointment sample are effectively separated. Moreover, the organic solvent is saved, the time consumption is short, the specificity is good, auxiliary materials do not interfere with tacrolimus impurity detection, and the impurity recovery rate also meets the requirements. The method is particularly suitable for effectively separating tacrolimus and related substancesfrom a complex matrix of tacrolimus ointment.

Description

technical field [0001] The invention relates to the field of drug analysis, in particular to the application of a solid-phase extraction column in the analysis of impurities in tacrolimus ointment. Background technique [0002] Tacrolimus, also known as FK506, is a fermentation product isolated from Streptomyces genus (streptomyces tsukubaensis) in 1985, and its chemical structure belongs to 23-membered macrolide antibiotics. Researched and developed by Fujisawa Corporation of Japan (now Astellas Pharmaceutical Co., Ltd.), as a powerful new immunosuppressant, it mainly suppresses the function of T lymphocytes by inhibiting the release of interleukin-2 (L-2) , 100 times stronger than cyclosporine (CsA). In recent years, as a first-line drug for liver and kidney transplantation, it has been marketed in 14 countries including Japan and the United States. Clinical experiments have shown that it has a good curative effect in heart, liver, kidney, bone marrow and other transplan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 陶艳黄和意黎文建柳莹陈敏江文敏
Owner GUANGZHOU MEDCAN PHARMATECH
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