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CN-121978229-A - Liquid phase detection method for dissolution rate of allopurinol tablet

CN121978229ACN 121978229 ACN121978229 ACN 121978229ACN-121978229-A

Abstract

The invention discloses a method for measuring dissolution rate and dissolution curve of a purine tablet, which uses high performance liquid chromatography to replace the current method for detecting the dissolution rate of the allopurinol tablet by using an ultraviolet spectrophotometer. The method uses a chromatographic column as a silica gel bonded octadecylsilane chemically bonded column, uses an acid solution-organic phase as a mobile phase, and adopts an isocratic elution mode for detection. The method for detecting the dissolution rate and the dissolution curve of the allopurinol tablet by using the high performance liquid chromatography can simply and conveniently finish detection, has the advantages of strong specificity, high accuracy and good repeatability, has application and linearity, and can efficiently and quickly detect the dissolution rate and the dissolution curve of the allopurinol tablet.

Inventors

  • CHEN QIMING
  • XU DAN
  • GUO XIA

Assignees

  • 万全万特制药（厦门）有限公司

Dates

Publication Date
20260505
Application Date
20251211

Claims (9)

  1. 1. A liquid phase detection method for allopurinol tablet dissolution adopts high performance liquid chromatography, wherein a chromatographic column is a silica gel bonded octadecylsilane column, and an acid solution-organic phase is used as a mobile phase for isocratic elution.
  2. 2. The method for detecting the dissolution rate of allopurinol tablets according to claim 1, wherein the chromatographic column is selected from one of the following silica gel-bonded octadecylsilane chemically bonded columns, promosil C and BDS HYPERSIL C.
  3. 3. The liquid phase detection method of the dissolution rate of the allopurinol tablet according to claim 1, wherein the acid solution is selected from one of a 0.1125% phosphoric acid solution, a 0.125% phosphoric acid solution and a 0.1375% phosphoric acid solution.
  4. 4. The method for detecting the dissolution rate of the allopurinol tablet according to claim 1, wherein the elution process is isocratic elution of 0.125% phosphoric acid solution-methanol (90:10).
  5. 5. The liquid phase detection method of allopurinol tablet dissolution rate according to claim 1, wherein the chromatographic column is preferably 150mm in length, 4.6mm in diameter and 5 μm in filler particle diameter.
  6. 6. The liquid phase detection method of allopurinol tablet dissolution according to claims 1 and 3, wherein the required acid solution with a certain proportion is preferably 0.125% phosphoric acid solution.
  7. 7. The liquid phase detection method of allopurinol tablet dissolution according to claims 2 and 5, wherein the chromatographic column is preferably BDS HYPERSIL C18.
  8. 8. The liquid phase detection method of the allopurinol tablet dissolution rate comprises the following steps of ① setting the flow rate to be 0.9-1.1 ml/min, ② setting the detection wavelength to be 265-275nm, and ③ chromatographic column temperature to be 30-40 ℃.
  9. 9. The liquid phase detection method of allopurinol tablet dissolution rate according to claim 8, wherein chromatographic conditions are ① flow rate is preferably 1.0ml/min, ② wavelength is preferably 270nm, and ③ column temperature is preferably 35 ℃.

Description

Liquid phase detection method for dissolution rate of allopurinol tablet Technical Field Through exploratory research, an allopurinol tablet dissolution HPLC measuring method is established, and research on related varieties is provided, and the dissolution items of medicines can be focused by referring to the planning method. Background Allopurinol, named Allopurinol in english, also known as allopurinol, isopurinol, is a xanthine oxidase inhibitor. Allopurinol has the chemical name of 4-hydroxypyrazolo [3,4-d ] pyrimidine, the chemical formula of C 5H4N4 O and the molecular weight of 136.11. The structural formula is as follows: allopurinol was approved for medical use in the united states in 1996. This medication is the most commonly prescribed drug in rank 40 of the united states in 2021, with the number of prescriptions prescribed in the current year exceeding 1500 tens of thousands. The absorbance of the ultraviolet spectrophotometry is accurate within the range of 0.3-0.7, and meanwhile, the two-step dilution preparation workload of the sample solution in the process of the dissolution curve detection experiment is huge, so that great working strength is brought to judging bioequivalence and evaluating the difference of the performances of the medicine in the in-vivo environment. Therefore, the method for measuring the dissolution rate of the allopurinol tablet by HPLC is of great significance in the aspect of the whole process research of the drug entering the liquid and the quality control of the pharmaceutical preparation. Disclosure of Invention The invention provides a liquid phase detection method for the dissolution rate of an allopurinol tablet, which can rapidly, effectively, simply and conveniently complete detection, solves the problem of huge workload of two-step dilution preparation of a sample solution in the dissolution curve detection experiment process, and further realizes the judgment of the bioequivalence of the allopurinol tablet and the evaluation of the performance of a medicine in an in-vivo environment. The invention provides a liquid phase detection method for the dissolution rate of an allopurinol tablet, which adopts high performance liquid chromatography, wherein a chromatographic column is a silica gel bonded octadecylsilane chemically bonded column, and an acid solution with a certain proportion is taken as a mobile phase A and an organic phase is taken as a mobile phase B for isocratic elution. The invention provides a liquid phase detection method for the dissolution rate of allopurinol tablets, wherein the isocratic elution program is 0.125% phosphoric acid solution-methanol (90:10). Preferably, the proportion of acid solution is a 0.125% phosphoric acid solution. Preferably, the column is provided as BDS HYPERSIL C (4.6 mm. Times.150 mm,5 μm). The dissolution HPLC determination method of the invention can be realized according to the following method: 1) Precisely weighing allopurinol reference substance 10mg, placing into a 10 ml measuring flask, adding 0.1 mo1/L sodium hydroxide solution 4m1, dissolving for 1min by ultrasound, diluting with water to scale, shaking, precisely weighing 5ml, placing into a 50ml measuring flask, diluting with 0.1NHC1 solution to scale, shaking; 2) The elution conditions were such that 1000ml of phosphate buffer solution at pH6.8 was used as the elution medium, the rotation speed was 75 revolutions per minute, the temperature was 37℃and the sample was sampled over 30 minutes. Taking a proper amount of dissolved solution, filtering, and taking a subsequent filtrate as a sample solution; 3) Setting the flow rate of the mobile phase to be 0.9-1.1 mL/min, preferably setting the flow rate of the mobile phase to be 1.0mL/min, setting the detection wavelength to be 265-275 nm, setting the optimal detection wavelength to be 270nm, setting the temperature of a column temperature box to be 30-40 ℃, and setting the temperature of the column temperature box to be 35 ℃ optimally; 4) About 50mg of allopurinol reference substance is put into a 50mL measuring flask, 10 mL of 0.1N sodium hydroxide solution is added, the solution is oscillated for 10min, water is used for diluting to scale, the solution is evenly shaken and filtered, 3.2mL, 3.6mL, 4mL, 4.4mL and 4.8mL are respectively measured precisely and put into a 200mL measuring flask as allopurinol reference mother solution, the solution is diluted to scale by mobile phase, and the solution is evenly shaken to obtain solutions with relative concentrations of 80%, 90%, 100%, 110% and 120% respectively; 5) Taking a reference substance solution and a test substance solution, placing at room temperature, and sampling at 0,2, 4, 6, 8 and 12 hours respectively; 6) 10. Mu.l of each of the above sample solutions was poured into a liquid chromatograph to complete the measurement. High performance liquid chromatograph, agilent 1260 InfinityII; Column BDS HYPERSIL C (4.6 mm. Times.150 mm,5 μm); mobile phase