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Wujin Linchuan Chemical

Determination of nabumetone and its preparation by high performance liquid chromatography

Abstract: Nabumetone is a new type of anti-inflammatory, antipyretic and analgesic with broad-spectrum anti-inflammatory effects. It has acute and chronic inflammation, rheumatoid arthritis, rheumatoid arthritis, osteoarthritis and soft tissue injury. Higher activity. In this paper, the content of nabumetone and its preparations were determined by reversed-phase high performance liquid chromatography with theophylline as the internal standard. The experimental results show that the method can effectively separate impurities, and the operation is simple, the reproducibility is good, and the results are accurate and reliable.

1 instrument and reagent Shimadzu LC-10A high performance liquid chromatography; SPD-10A adjustable wavelength detector; C-R7Aeplus data processor.

Nabumetone ketone reference substance (content 99.85%), raw materials, Southwest Synthetic Pharmaceutical Factory; theophylline, China National Institute for the Control of Pharmaceutical and Biological Products; nabumetone tablets, Jiangxi Liming Pharmaceutical Factory. Methanol, sodium acetate and glacial acetic acid were all analytically pure; water was distilled water.

2 Chromatographic conditions column: Shimadzu Shim-packCLC-ODS column, 150mm × 4.6mm; mobile phase: methanol -0.05mol.L-1 acetate buffer (0.05mol.L-1 sodium acetate solution with glacial acetic acid pH was 3.5) (65:35); flow rate: 1.0 mL.min-1; detection wavelength: 254 nm; injection amount: 10 μL.

The chromatogram of nabumetone and internal standard under the above chromatographic conditions is shown in Figure 1.

3 Linear relationship The nabumetone was accurately weighed and the amount of theophylline in the internal standard was determined by using methanol to prepare a solution of 1.08 mg.mL-1 and 1.05 mg.mL-1, respectively. Precisely measure the reference solution 2.0, 3.0, 4.0, 5.0, 6.0, 7.0, 8.0mL into a 25mL volumetric flask, each precision added 5mL of the internal standard solution, dilute to the mark with methanol, shake, and measure the injection. The results showed that the peak area ratio of nabumetone concentration in the range of 86.4~345.6μg.mL-1 showed a good linear relationship with the sample concentration. The regression equation (n=7) was: Y=3.43×10-3 5.64×10 -3Xr=0.99981. Theophylline (1.88min) 2. Nabumetone (3.75min)

4 Sample determination 4.1 Determination of the content of the raw materials Weigh accurately about 100mg of the sample, placed in a 100mL volumetric flask, dissolved in methanol and diluted to the mark. Accurately draw 5mL into a 25mL volumetric flask, accurately add 5mL of the internal standard solution, dilute to the mark with methanol, shake well, and measure the injection. The content was calculated by the internal standard method. The results of the three batches of raw materials are shown in Table 1.

Sample labeled amount %RSD/%199.470.5299.680.7399.450.7 Table 1 Determination of raw material content (n=3)

4.2 Determination of tablet content Take 20 tablets, accurately weighed, finely weighed, accurately weighed the appropriate amount (corresponding to about 500 mg of nabumetone), placed in a 500 mL volumetric flask, dissolved in methanol and diluted to the mark, shake well , filtered. Accurately draw 5mL of the continuous filtrate into a 25mL volumetric flask, accurately add 5mL of the internal standard solution, add methanol to the mark, shake well, and measure the sample.

The results of the three batches of samples are shown in Table 2.

Sample labeling amount%RSD/%195.890.7297.660.43100.00.65 Discussion 5.1 The authors weighed the adjuvant and nabumetone reference substance according to the prescription ratio of nabumetone tablets, and conducted the recovery test. The average recovery rate of the 5 determination results. It is 99.46% and the RSD is 0.6%. The test proves that this method uses theophylline as the internal standard, which can improve the reproducibility of the analysis results, avoid the systematic error caused by the injection and instrument factors, and avoid the error caused by the ultraviolet spectrophotometry of impurities and auxiliary materials. .

5.2 The amount of methanol added in the mobile phase and the pH of the mobile phase have a significant effect on the internal standard, especially on the peak time and peak shape of the sample. The larger the amount of methanol added and the lower the pH, the faster the peak time and the improved peak shape. After many experiments, the mobile phase with methanol-0.05mol.L-1 acetate buffer (65:35, pH3.5) is better, the peak is fast, the peak shape and resolution are good, and the result is satisfactory. .

5.3 The solution of this product is placed in a colorless and transparent measuring bottle. After being placed for 1 week, the ratio of the peak area of ??the sample to the internal standard is basically unchanged, and the solution is stable.

(Source: China Chemical Instrument Network)

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