A method for determining the content of pranlukast
By optimizing the mobile phase and chromatographic conditions of high-performance liquid chromatography, the problem of peak tailing in the determination of prolansta content was solved, achieving accurate and reproducible content determination and ensuring the quality control of the active pharmaceutical ingredient.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- JIANCHUANG PORT (HAINAN) TECHNOLOGY CO LTD
- Filing Date
- 2026-05-16
- Publication Date
- 2026-07-24
AI Technical Summary
Existing liquid chromatography detection methods for determining prencalfloxacin often result in peak tailing or peak asymmetry, leading to inaccurate peak area integration. This affects the precision and accuracy of content determination and fails to meet the quality control requirements of the active pharmaceutical ingredient.
High performance liquid chromatography (HPLC) was used with a silica-bonded octadecylsilane column. Mobile phase A was phosphate buffer containing sodium heptanesulfonate, and mobile phase B was chromatographically pure acetonitrile. Isocratic elution was performed, and the mobile phase ratio and chromatographic conditions were optimized. The ultraviolet absorption wavelength was 285 nm.
It improved the chromatographic peak symmetry of prunlast, enhanced the accuracy and reproducibility of content determination, and ensured the quality control of the active pharmaceutical ingredient.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of chemical drug and food analysis technology, specifically to a detection method for determining the content of pramuxat raw material using liquid chromatography. Background Technology
[0002] Allergic diseases such as asthma are common chronic respiratory illnesses that severely impact patients' quality of life, and in some severe cases, acute attacks can be life-threatening. Current research data indicates that Pranlukast, a cysteyl leukotriene receptor antagonist, has targeted therapeutic effects and is widely used clinically for the treatment of allergic diseases.
[0003] Prenstar, with the molecular formula C27H23N3O4 and a molecular weight of 453.49: Its chemical structural formula is as follows:
[0004] In the synthesis of pramuxata, quality analysis is crucial for content control. An accurate method for determining pramuxata content can guide and monitor the synthesis process, improving the yield and purity of the final product. Therefore, it has significant practical implications for quality control in the pramuxata synthesis process. Existing liquid chromatography methods for determining pramuxata often exhibit peak tailing or peak asymmetry, leading to inaccurate peak area integration and affecting the precision and accuracy of content determination, failing to meet the stringent quality control requirements for active pharmaceutical ingredients. Summary of the Invention
[0005] This invention proposes a method for determining the content of pramuxartin, which enables rapid, effective, and accurate determination of pramuxartin content, thereby achieving quality control of the final product, the active pharmaceutical ingredient.
[0006] This invention proposes a method for determining the content of prancelast using high performance liquid chromatography (HPLC). The chromatographic column is a silica-bonded octadecylsilane column, mobile phase A is a phosphate buffer containing sodium heptanesulfonate, and mobile phase B is chromatographically pure acetonitrile, with isocratic elution.
[0007] Preferably, the phosphate buffer solution is a 20 mM sodium dihydrogen phosphate solution, with the pH adjusted to 2.8 using phosphoric acid or sodium hydroxide; the concentration of sodium heptanesulfonate in the phosphate buffer solution is 5 mM.
[0008] Preferably, the mobile phase is a mixture of solution A and acetonitrile in a volume ratio, wherein solution A is a solution of sodium dihydrogen phosphate buffer containing heptanesulfonate and acetonitrile premixed in a ratio of 60:40 (v / v); the mobile phase ratio is solution A:acetonitrile = 80:20, 70:30, 60:40 or 50:50 (v / v).
[0009] Preferably, the chromatographic column is a silica-bonded octadecylsilane column (250 mm × 4.6 mm, 5 μm).
[0010] The analytical method described in this invention can be tested according to the following method: Example 1: Mobile phase ratio 80:20 Diluent: Solution A (20mM sodium dihydrogen phosphate buffer containing 5mM heptanesulfonate, pH 2.8): acetonitrile = 60:40; System suitability solution: Take an appropriate amount of pramlast, add diluent to dissolve it and prepare a solution containing 0.5 mg of pramlast per 1 ml; The designed mobile phase flow rate is 1.0 mL / min, the UV wavelength is 285 nm, the column oven temperature is 35 °C, and the injection volume is 10 μl. Elution method: isocratic elution (solution A: acetonitrile = 80:20); High performance liquid chromatograph: Waters e2695; Accurately measure 10 μl of the above solution, inject it into the liquid chromatograph, and record the chromatogram.
[0011] Example 2: Mobile phase ratio 70:30 Diluent: Same as in Example 1; System suitability solution: Same as in Example 1; The designed mobile phase flow rate is 1.0 mL / min, the UV wavelength is 285 nm, the column oven temperature is 35 °C, and the injection volume is 10 μl. Elution method: isocratic elution (solution A: acetonitrile = 70:30); High performance liquid chromatograph: Waters e2695; Accurately measure 10 μl of the above system suitability solution, inject it into the liquid chromatograph, and record the chromatogram.
[0012] Example 3: Mobile phase ratio 60:40 Diluent: Same as in Example 1; System suitability solution: Same as in Example 1; The designed mobile phase flow rate is 1.0 mL / min, the UV wavelength is 285 nm, the column oven temperature is 35 °C, and the injection volume is 10 μl. Elution method: isocratic elution (solution A: acetonitrile = 60:40); High performance liquid chromatograph: Waters e2695; Accurately measure 10 μl of the above system suitability solution, inject it into the liquid chromatograph, and record the chromatogram.
[0013] Example 4: Mobile phase ratio 50:50 Diluent: Same as in Example 1; System suitability solution: Same as in Example 1; The designed mobile phase flow rate is 1.0 mL / min, the UV wavelength is 285 nm, the column oven temperature is 35 °C, and the injection volume is 10 μl. Elution method: isocratic elution (solution A: acetonitrile = 50:50); High performance liquid chromatograph: Waters e2695; Accurately measure 10 μl of the above system suitability solution, inject it into the liquid chromatograph, and record the chromatogram.
[0014] This invention employs a silica-bonded octadecylsilane column, with mobile phase A being phosphate buffer containing sodium heptanesulfonate and mobile phase B being acetonitrile. The chromatographic conditions, including an ultraviolet absorption wavelength of 285 nm, effectively improve the peak symmetry of pransilactone, enabling accurate determination of pransilactone content. This invention utilizes an HPLC analysis method to solve the peak tailing problem in pransilactone content determination, thereby improving the accuracy and reproducibility of the results and ensuring the quality control of pransilactone raw material. Attached Figure Description
[0015] Figure 1 This is the HPLC chromatogram for Example 1; Figure 2 This is the HPLC chromatogram for Example 2; Figure 3 This is the HPLC chromatogram for Example 3; Figure 4 This is the HPLC chromatogram for Example 4. Detailed Implementation
[0016] The following embodiments are provided to further understand the present invention, but are not limited to the scope of these embodiments.
[0017] Instruments and conditions used in the examples: High performance liquid chromatograph: Waters e2695; Column: Silica-bonded octadecylsilane column (250 mm × 4.6 mm, 5 μm); Mobile phase A: 20 mM sodium dihydrogen phosphate buffer (pH 2.8) containing 5 mM heptanesulfonate:acetonitrile = 60:40; Mobile phase B: acetonitrile; Column oven temperature: 35 °C; Injection volume: 10 μl; UV wavelength: 285 nm; Elution method: isocratic elution.
[0018] Figure 1Solution preparation: Take an appropriate amount of pranoxetine, add diluent to dissolve it and prepare a system-suitable solution containing 0.5 mg of pranoxetine per 1 ml. Perform high performance liquid chromatography analysis under the above conditions (mobile phase ratio 80:20) and record the chromatogram. The results show that the main peak of pranoxetine is symmetrical, the tailing factor is close to 1.0, and the theoretical plate number meets the requirements for content determination.
[0019] Figure 2 Solution preparation: Same as above Figure 1 High performance liquid chromatography (HPLC) analysis was performed under the above conditions (mobile phase ratio 70:30), and the chromatogram was recorded. The results showed that the retention time of the main peak of prenstarst was moderate, and the peak shape was sharp and symmetrical, which met the precision requirements for content determination.
[0020] Figure 3 Solution preparation: Same as above Figure 1 High performance liquid chromatography (HPLC) analysis was performed under the above conditions (mobile phase ratio 60:40), and the chromatogram was recorded. The results showed that the main peak of prenstard had good separation and no peak tailing, making it suitable for routine content determination.
[0021] Figure 4 Solution preparation: Same as above Figure 1 High-performance liquid chromatography (HPLC) analysis was performed under the above conditions (mobile phase ratio 50:50), and the chromatogram was recorded. The results showed that the main peak of prenstarst eluted quickly, and the peak shape still maintained good symmetry, proving that the method is still effective under high organic phase ratio.
[0022] from Figures 1-4 This indicates that the method of the present invention, using the same HPLC analysis method, can effectively improve the chromatographic peak shape of pranstar, achieve accurate and precise determination of its content, and thus effectively control the product quality of pranstar.
Claims
1. A method for determining the content of pralidoxetine, employing high performance liquid chromatography, characterized in that, The chromatographic column is a silica-bonded octadecylsilane column, with a UV detector. The mobile phase consists of a phosphate buffer solution containing the ion-pairing reagent sodium heptanesulfonate and the organic solvent acetonitrile, and isocratic elution is performed. By optimizing the mobile phase composition, the chromatographic peak symmetry of prenstar is improved, enabling accurate determination of its content.
2. The analytical method according to claim 1, characterized in that, The phosphate buffer solution is a 20 mM sodium dihydrogen phosphate solution, with the pH adjusted to 2.8 using phosphoric acid or sodium hydroxide.
3. The analytical method according to claim 1, characterized in that, The ion-pairing reagent is sodium heptanesulfonate at a concentration of 5 mM in phosphate buffer.
4. The analytical method according to claim 1, characterized in that, The organic solvent is chromatographically pure acetonitrile.
5. The analytical method according to claim 1, characterized in that, The mobile phase is composed of solution A and acetonitrile in a volume ratio, wherein solution A is a solution of sodium dihydrogen phosphate buffer containing heptanesulfonate as described in claim 3 and acetonitrile in a 60:40 (v / v) ratio.
6. The analytical method according to claim 5, characterized in that, The mobile phase ratio for isocratic elution is any one of the following: Solution A : Acetonitrile = 80 : 20 (v / v) Solution A : Acetonitrile = 70 : 30 (v / v) Solution A : Acetonitrile = 60 : 40 (v / v) Solution A : Acetonitrile = 50 : 50 (v / v).
7. The analytical method according to claim 1, characterized in that, The chromatographic column has a length of 250 mm, a diameter of 4.6 mm, and a packing particle size of 5 μm.
8. The analytical method according to claim 1, characterized in that, The detection wavelength is 285nm.
9. The analytical method according to claim 1, characterized in that, Chromatographic conditions include: flow rate of 0.5-1.5 mL / min, column temperature of 30-50℃, and injection volume of 5-20 μL.
10. The analytical method according to claim 9, characterized in that, The optimized chromatographic conditions are as follows: flow rate of 1.0 mL / min, column temperature of 35 °C, and injection volume of 10 μL.