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A method for simultaneous detection of rimonabant and sibutramine

A technology of rimonabant and detection wavelength, applied in the field of simultaneous detection of rimonabant and sibutramine, can solve the problems of single detection method, complicated and unfavorable on-site detection, etc., and achieves simple operation, fast analysis speed, and results. Reliable and responsive effects

Inactive Publication Date: 2011-12-07
SHANGHAI INST OF MEASUREMENT & TESTING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The technical problem to be solved by the present invention is in order to overcome the defects such as single, multifarious and unfavorable on-site detection of existing detection methods for rimonabant and sibutramine, and proposes a method for simultaneously detecting rimonabant and sibutramine. Proven HPLC method

Method used

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  • A method for simultaneous detection of rimonabant and sibutramine
  • A method for simultaneous detection of rimonabant and sibutramine
  • A method for simultaneous detection of rimonabant and sibutramine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1 standard curve

[0029] 1. Sample preparation

[0030] Standard stock solution: Accurately weigh 0.0200 g each of rimonabant and sibutramine reference substances into two 10mL volumetric flasks, add methanol to dissolve and dilute to the mark, shake well, and obtain a reference substance reserve with a concentration of 2mg / mL Stored in a -20°C refrigerator, the validity period is one year.

[0031] Mixed standard working solution: Accurately measure the appropriate amount of each standard stock solution, dilute with methanol to make a series of mixed standard working solutions with a concentration of 0.01, 0.05, 0.1, 1, 2, 5, 10, and 20 μg / mL, and store them in a refrigerator at 4 °C. Valid for six months.

[0032] 2. Chromatographic method

[0033] A series of mixed standard working solutions were injected into the chromatographic system with an injection volume of 10 μL, the column temperature was 20 ° C, methanol was used as the mobile phase, and the ...

Embodiment 2

[0041] Embodiment 2 precision experiment

[0042] Shake the 10 μg / mL mixed standard working solution prepared in Example 1, inject 10 μL each time, repeat the injection 6 times, and analyze according to the HPLC conditions in Example 1. The peak area A was measured each time, and the RSDs were 1.47% and 1.25% (n=6), respectively, indicating that the precision was good. See Table 2 for relevant data.

[0043] Table 2 Precision experimental data (n=6)

[0044] compound

Embodiment 3

[0045] Embodiment 3 Stability experiment

[0046] Take the mixed standard working solution with the same concentration of 5 μg / mL, place it at room temperature for 0, 1, 2, 4, 6, 8, 12, and 24 hours, and then inject samples sequentially for determination, and measure the peak areas of rimonabant and sibutramine respectively , quantified by external standard method, calculated its concentration, RSD were 2.62%, 2.13%, indicating that rimonabant and sibutramine solution at room temperature within 24h good stability. See Table 3 for relevant data.

[0047] Table 3 Stability experimental data

[0048] time (h)

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Abstract

The invention discloses a method for simultaneously detecting rimonabant and sibutramine, which comprises the following steps of: preprocessing a sample to be detected, and detecting by using high performance liquid chromatography, wherein the chromatographic conditions of the high performance liquid chromatography are that: a chromatographic column takes octadecylsilane chemically bonded silica as a filler, methanol or acetonitrile is taken as a mobile phase for isocratic elution, and the detection wavelength is 220-225nm. The detection method has the advantages of simple operation, high analysis speed and reliable and sensitive results, and the quality control of a product can be realized by simultaneously detecting and monitoring the rimonabant and the sibutramine.

Description

technical field [0001] The invention relates to a method for simultaneously detecting rimonabant and sibutramine. Background technique [0002] With the unreasonable dietary structure caused by the continuous improvement of people's living standards in our country, the number of obese people has increased year by year, followed by the continuous increase of the potential number of diabetes, hypertension and cardiovascular diseases, so it has the function of weight loss Food became the center of attention. However, in order to enhance the "quick-acting" and "strong-acting" weight-loss effects, some unscrupulous manufacturers illegally add western medicine ingredients to functional foods. The amount of addition is often determined randomly, which may endanger the health of consumers. Wherein rimonabant and sibutramine are two commonly used antipsychotic additive drugs: rimonabant (shown in formula 1) was first proposed by Barth et al. (U.S.Patent No.5624941 and EP 0656354), ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 刘刚李兰英任淑贞张波龚飞雁丁敏邱旸
Owner SHANGHAI INST OF MEASUREMENT & TESTING TECH
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