Detection control method of new impurities in tramadol hydrochloride preparation and obtained impurity
A tramadol hydrochloride, detection and control technology, applied in chemical instruments and methods, measuring devices, preparation of organic compounds, etc., can solve the problem that the detection method cannot effectively detect and separate new impurities, so as to provide separation effect and detection Effect, increased safety, good separation effect
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Embodiment 1
[0046] A method for detection and control of new impurities in tramadol hydrochloride preparations, comprising the following steps:
[0047] (1) Take 200 mg of tramadol hydrochloride, add mobile phase, the mobile phase uses solution A: acetonitrile (77:23) as the mobile phase, wherein solution A measures 950 ml of water, puts it in a 1000 ml measuring bottle, and adds perchloric acid 5ml, 4ml of 25% ammonia water, dilute to the mark with water, shake well, adjust the pH value to 2.2±0.2 with 25% ammonia water or perchloric acid to prepare, ultrasonic for 5 minutes to dissolve tramadol hydrochloride, dilute to make 1ml The solution containing 4 mg of tramadol hydrochloride in the medium is shaken up, filtered through a 0.45 μm filter membrane, and the subsequent filtrate is taken as the test solution, as the test preparation to be tested in the present invention, for detecting and further controlling impurities in the test preparation ;
[0048] (2) Get 25 mg of tramadol hydro...
Embodiment 2
[0062] The present invention is to the new impurity carboxymethyl tramadol obtained by the detection control method of the new impurity in the tramadol hydrochloride preparation of embodiment 1, chemical name 2-((2-((dimethylamino)methyl)- 1-(3-methoxyphenyl)cyclohexyl)oxy)acetic acid, the chemical structural formula is as follows:
[0063]
[0064] The present invention obtains such as by the above-mentioned detection method of embodiment 1 image 3 The detected content peak diagram of carboxymethyl tramadol and other impurities is shown.
[0065] The present invention also detects the impurity content by comparing the old method 1 and the old method 2 of the known liquid chromatography of Table 1 with the method of the present invention, and obtains respectively as follows figure 1 and figure 2 Shown collection of illustrative plates and the method step of the present invention and parameters etc. are set and obtain image 3 compared graphs.
[0066] Known method of...
Embodiment 3
[0086] A method for detection and control of new impurities in tramadol hydrochloride preparations, the difference from Example 1 is that the amount taken is different,
[0087] (1) get tramadol hydrochloride preparation to be tested, add mobile phase, dilute and make the solution containing tramadol hydrochloride 3mg in every 1ml;
[0088] (2) get tramadol hydrochloride reference substance, add 0.1mol / L hydrochloric acid solution to dissolve and dilute to make the stock solution containing tramadol hydrochloride 0.4mg in every 1ml;
[0089] (3) Get carboxymethyl tramadol reference substance, dissolve and dilute with 0.1mol / L hydrochloric acid solution and make the stock solution that contains 0.1mg in every 1ml;
[0090] (4) get the fine powder and impurity A (impurity I) of tramadol hydrochloride preparation under step (1) assay item with mobile phase, make the mixed solution containing tramadol hydrochloride 3mg and impurity A 7 μ g in every 1ml as System suitability solut...
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