Gas chromatographic analysis method for methane triethyl tricarboxylate related substances
A technology of gas chromatography analysis and methanetricarboxylic acid, which is applied in the direction of analyzing materials, material separation, measuring devices, etc., can solve the problem that production, research and development and purification have no substantial guiding role, impurities cannot be effectively separated and analyzed, and cannot be accurately quantified Determination of impurities and other issues to achieve objective product quality, great positive effect, and good durability
Active Publication Date: 2022-01-28
南京锐志生物医药有限公司
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Problems solved by technology
That is to say, the impurities described in the present invention cannot be effectively separated and analyzed under the above conditions, and these potential impurities cannot be accurately quantitatively determined.
Such a related substance analysis method cannot separate the potential impurities of triethyl methanetricarboxylate very well, and the obtained results are not accurate, and have no substantial guiding effect on production, research and development and purification
Method used
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Embodiment 1
[0052] Gas chromatographic analysis method detects related substances in triethyl methanetricarboxylate, specifically comprises the following steps:
[0053] (1) Chromatographic condition setting:
[0054] Chromatographic column: capillary column with (5%-phenyl)-methylpolysiloxane as stationary liquid, size 30m×0.32mm×0.25μm;
[0055] Column temperature: the initial temperature is 40°C, the temperature is raised to 55°C at a rate of 3°C per minute, and then raised to 220°C at a rate of 8°C per minute, and maintained for 5 minutes;
[0056] Injection port temperature: 280°C;
[0057] Detector: hydrogen flame ionization detector (FID), the detector temperature is 300 ℃;
[0058] Carrier gas: nitrogen
[0059] Carrier gas flow rate: 1.5ml / min;
[0060] Injection volume: 1μl;
[0061] Split ratio: 100:1;
[0062] (2) Preparation of the test solution: take an appropriate amount of trimethyl methanetricarboxylate, accurately weigh it, and dilute it with N,N-dimethylformamide ...
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The invention provides a gas chromatographic analysis method of methane triethyl tricarboxylate related substances. By selecting a proper chromatographic column and a detector, changing the temperature of a sample inlet, the temperature of a detector and a split ratio and designing a reasonable heating program, the diethyl malonate and other single impurities in the triethyl methanetricarboxylate related substances are accurately recognized, the separation effect is outstanding, the sensitivity, accuracy, precision, durability and the like of the method are good, and the method is simple to operate, is time-saving and efficient, and has greater positive progress effect and practical application value.
Description
technical field [0001] The invention relates to the technical field of drug analysis, in particular to a gas chromatography analysis method for related substances of triethyl methanetricarboxylate. Background technique [0002] Ketorolac tromethamine is a derivative of pyrrolidine carboxylic acid. As early as 1990, ketorolac tromethamine was approved abroad as a non-steroidal anti-inflammatory drug for perioperative analgesia. It is the only NSAIDs drug approved by PDA (Association for Parenteral Drugs) for postoperative analgesia. [0003] Triethyl methanetricarboxylate (Triethyl methanetricarboxylate) is one of the main raw materials for the synthesis of ketorolac tromethamine, and its synthetic route is as follows: [0004] [0005] The main impurity in triethyl methanetricarboxylate is diethyl malonate. If it is not controlled, it will be introduced into the final product, resulting in difficulties in refining the final product, difficult to reach quality control sta...
Claims
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IPC IPC(8): G01N30/02G01N30/06G01N30/30G01N30/32G01N30/34G01N30/68G01N30/86
CPCG01N30/02G01N30/06G01N30/30G01N30/32G01N30/34G01N30/68G01N30/8675G01N2030/324
Inventor 张倩颖徐丽汤婷婷万琴沙向阳
Owner 南京锐志生物医药有限公司