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HPLC detection method of tramadol hydrochloride impurity E

A tramadol hydrochloride and detection method technology, applied in the field of drug analysis, can solve problems such as complex developing solvent system, uncontrollable data, poor retention of impurity E, etc., and achieve easy product quality control, high accuracy and precision , good stability and reproducibility

Inactive Publication Date: 2020-09-25
SHANDONG XINHUA PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] (1) The development solvent system is complex, and when it is applied to the precursor reagents toluene, isopropanol, and ammonia water, inhalation is highly toxic to the body, has a strong smell, and seriously pollutes the environment;
[0017] (2) Sodium nitrite solution, Dragendorff reagent are complicated to prepare, and the operation is loaded down with trivial details;
[0018] (3) Observation with naked eyes has a large subjective error; the chromatographic results can only qualitatively analyze whether the sample contains impurity E, but cannot accurately quantitatively reflect the content of impurity E;
[0019] (4) It is difficult to save the experimental results of thin-layer chromatography, the data cannot be stored, and it is difficult to retrieve; there is a risk of uncontrollable data when applied to quality control in the mass production process
[0020] At present, the main limitation of impurity E in tramadol hydrochloride EP Pharmacopoeia is that the application of liquid chromatography and other instrumental analysis methods is weak in ultraviolet absorption, which shows that the signal response in liquid chromatography is not high and the sensitivity is low; impurity E has poor retention and peaks Fast, resulting in peak area may contain other miscellaneous peaks, inaccurate quantification, causing analysis errors

Method used

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  • HPLC detection method of tramadol hydrochloride impurity E
  • HPLC detection method of tramadol hydrochloride impurity E
  • HPLC detection method of tramadol hydrochloride impurity E

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] (1) Instrument: Shimadzu liquid chromatograph LC-20AT;

[0056] Chromatographic column: Agilent ZORBAX SB-Phenyl 4.6×250mm 5μm;

[0057] Mobile phase: 0.2% trifluoroacetic acid-acetonitrile (83:17) is the mobile phase;

[0058] Wavelength: 270nm;

[0059] Column temperature: 40°C;

[0060] Flow rate: 1.0ml / min;

[0061] Injection volume: 20ul.

[0062] (2) Determination method:

[0063] Precisely measure 20 μl of each solution, inject it into a liquid chromatograph, record the liquid chromatogram, and calculate the peak area according to the external standard method.

[0064] Table 1 Chromatographic peak positioning and resolution test results

[0065] Solution name name retention time (min) Peak area Reference solution Impurity E 4.414 2300 Spiked test solution Impurity E 4.334 2277

[0066] The results showed that the blank solution, the test solution and other impurities in the test did not interfere with the detection of im...

Embodiment 2

[0068] Implementation steps:

[0069] Solution preparation: Accurately weigh an appropriate amount of the impurity E reference substance, dissolve and dilute it with the mobile phase to make a solution with a concentration of about 200 μg / ml, and use it as the impurity E reference substance stock solution. Dilute step by step with the mobile phase to prepare a solution with a concentration of about 1 μg / ml, accurately measure 20 μl, inject it into the liquid chromatograph, record the chromatogram, and visually observe that the peak height of the impurity E chromatographic peak is about 3 times the baseline noise, which can be As the detection limit, the concentration of impurity E is about 1 μg / ml, which is equivalent to 0.005% of the concentration of the test solution;

[0070] Take the impurity E reference substance stock solution, dilute it step by step with the mobile phase, and prepare a solution with a concentration of about 2 μg / ml, accurately measure 20 μl, inject it i...

Embodiment 3

[0075] On the basis of the established chromatographic conditions, change the column temperature, change the flow rate, and change the ratio of the mobile phase, and accurately measure 20 μl each of the blank solvent and the spiked test solution, inject them into the liquid chromatograph, and record the chromatogram.

[0076] Table 3 Impurity E inspection durability test results

[0077]

[0078] The results showed that the separation between main peak and impurity, and between impurity and impurity was greater than 1.5 with small adjustment of column temperature and flow rate and replacement of chromatographic column, and the durability of the method was good. During the production process, slight changes in the detection environment will not affect the accuracy of the detection.

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Abstract

The invention provides an HPLC detection method for the tramadol hydrochloride impurity E. According to the invention, the impurity E in tramadol hydrochloride is detected through a liquid chromatography method, so the existence of the impurity E can be qualitatively analyzed, and the accurate content of the impurity E can be quantitatively analyzed. Compared with the existing TLC thin-layer chromatography method, the method is simpler and more convenient in experiment operation; chromatographic peaks are free of interference and high in sensitivity, and methodological verification results meet requirements; therefore, the detection method is good in specificity, high in sensitivity, accurate in quantification and less affected by the detection environment; the liquid chromatography detection method provided by the invention is more suitable for large-scale production and product quality control in a quality control process.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to a method for detecting related substances of tramadol hydrochloride. Background technique [0002] Tramadol hydrochloride (Tramadol), whose chemical name is (±)-trans-1-(m-methoxyphenyl)-2-(dimethylamino)-methyl)-cyclohexanol hydrochloride , molecular formula: C16H26ClNO2, molecular weight: 299.84. [0003] Its structural formula is: [0004] [0005] Tramadol is a powerful non-morphine analgesic. It mainly acts on specific receptors related to pain in the central nervous system. It does not cause smooth muscle spasm and obvious respiratory depression, it takes effect 10-20 minutes after oral administration, and the analgesic effect can last for 4-6 hours. May prolong the duration of barbiturate anesthesia. It can enhance the analgesic effect when used together with stable drugs. [0006] (2RS)-2-Dimethylaminomethylcyclohexanone ((2RS)-2-[(dimethylamino)-methyl]cyclohexanone...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/047
Inventor 李丹吴辉王付荣
Owner SHANDONG XINHUA PHARMA CO LTD
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