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Testing method for related substances of drug combination containing tegafur, gimeracil and oteracil potassium

A technology of oteracil potassium and gimeracil, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve problems such as difficult detection methods, and achieve scientific impurity calculation methods, shortened separation time, and good separation effects.

Active Publication Date: 2014-03-26
鲁南新时代生物技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Since it is a compound preparation of three components, it is difficult to establish a detection method for related substances in the S-1 drug composition
At present, there is no literature report on the detection method of related substances in the pharmaceutical composition of S-1

Method used

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  • Testing method for related substances of drug combination containing tegafur, gimeracil and oteracil potassium
  • Testing method for related substances of drug combination containing tegafur, gimeracil and oteracil potassium
  • Testing method for related substances of drug combination containing tegafur, gimeracil and oteracil potassium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Instruments and conditions: Waters 2695 liquid chromatography system, PDA detector, chromatographic column: Inertsil ODS-3 (4.6mm×150mm, 5μm); detection wavelength: 220mn; column temperature: 35°C; g of potassium dihydrogen phosphate is dissolved in water and diluted to 1800ml, add 4ml of 10% tetrabutylammonium hydroxide, mix well, adjust the pH value to 3.2 with phosphoric acid)-methanol (94:6) as mobile phase A, methanol-acetonitrile (7 : 1) is mobile phase B, and carries out linear gradient elution according to the following table.

[0035]

[0036] experiment procedure:

[0037] 1. Peak positioning test: Take 24.5 mg of oteracil potassium reference substance, 25.1 mg of tegafur reference substance, 7.3 mg of gimeracil reference substance, and 7.2 mg of impurity A reference substance, weigh them accurately, and put them in the same 100ml measuring bottle. Add 30% acetonitrile aqueous solution (pH11.2) to dissolve and dilute to the mark, shake well, measure accord...

Embodiment 2

[0051] Instruments and conditions: Agilent 1200 liquid chromatography system, VWD detector, chromatographic column: Inertsil ODS-3 (4.6mm×150mm, 5μm); detection wavelength: 220nm; column temperature: 35°C; g of potassium dihydrogen phosphate is dissolved in water and diluted to 1800ml, add 4ml of 10% tetrabutylammonium hydroxide, mix well, adjust the pH value to 3.2 with phosphoric acid)-methanol (94:6) as mobile phase A, methanol-acetonitrile (7 : 1) is mobile phase B, and carries out linear gradient elution according to the following table.

[0052]

[0053] Test procedure: Take appropriate amounts of Tegafur, Gimeracil, Oteracil Potassium, and Impurity A reference substance respectively, and accurately weigh them to make concentrations of 1.00 μg / ml, 0.29 μg / ml, 0.98 μg / ml, and 0.29 μg The mixed solution of the reference substance per ml was diluted according to the stepwise dilution method, and the quantification limits and detection limit. The limit of quantification...

Embodiment 3

[0056] Instruments and conditions: Waters 2695 liquid chromatography system, PDA detector, chromatographic column: Welch Materials C18 (4.6mm×250mm, 5μm); detection wavelength: 220nm; column temperature: 35°C; phosphate buffer (take 1.3g Dissolve potassium dihydrogen phosphate in water and dilute to 1800ml, add 4ml of 10% tetrabutylammonium hydroxide, mix well, adjust the pH value to 3.2 with phosphoric acid) as mobile phase A, methanol-acetonitrile (1:1) as mobile phase B, Carry out linear gradient elution according to the table below.

[0057]

[0058]

[0059] Test procedure: Take 104.6mg of the accelerated 12-month sample of S-1 capsule, put it in a 25ml measuring bottle, add 30% acetonitrile aqueous solution (pH 11.2) to dissolve and dilute to the mark, shake well, filter, and measure according to the law.

[0060] As can be seen from the test results: the detection method of the present invention can separate the main peaks of the S-Gio Capsules and its impurity pe...

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Abstract

The invention relates to a testing method for the related substances of drug combination containing tegafur, gimeracil and oteracil potassium. The testing method adopts the high-efficiency liquid chromatography (gradient elution) to carry out a test, the stationary phase is a chromatographic column with octyl or octadecyl-bonded silica gel as filler, the mobile phase A is saline solution containing ion-pair reagent or the mixture of the saline solution and any one or both of methanol and acetonitrile, the mobile phase B is any one of acetonitrile and methanol or the mixture of acetonitrile and methanol, and solvent is 10 to 90 percent of aqueous acetonitrile solution, the pH of which is 10.5 to 11.5. The testing method has the advantages of good separation effect, high sensitivity, high operability and the like, and not only can increase the level of tests on the related substances of the tegafur, gimeracil and oteracil potassium drug combination but also enhances the quality control of the combination.

Description

technical field [0001] The invention relates to a method for detecting related substances of a pharmaceutical composition containing tegafur, gimeracil and oteracil potassium. Background technique [0002] The active ingredients of the S-1 compound are composed of tegafur (FT), gimeracil (CDHP) and oteracil potassium (OXO). Its mechanism of action is: after oral administration, FT is gradually converted into 5-fluorouracil (5-FU) in the body. ℃DHP selectively and reversibly inhibits the 5-FU catabolic enzyme DPD present in the liver, thereby increasing the concentration of 5-FU from FT. With the increase of 5-FU concentration in the body, the 5-FU phosphorylation product-5-fluoronucleotide in tumor tissue can maintain a high concentration, thereby enhancing the anti-tumor effect. After oral administration, OXO is distributed in the gastrointestinal tract, and can selectively and reversibly inhibit orotate phosphoribosyltransferase, thereby selectively inhibiting the conver...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/36
Inventor 赵志全刘阿利吴善霞
Owner 鲁南新时代生物技术有限公司
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