GC method for detecting residual quantity of solvent in compound

A technology for analyzing compounds and solvents, used in measuring devices, instruments, scientific instruments, etc., and can solve problems such as half-life extension

Active Publication Date: 2014-04-16
NEW FOUNDER HLDG DEV LLC +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Most products have extended half-life, such as gatifloxacin and moxifloxacin

Method used

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  • GC method for detecting residual quantity of solvent in compound
  • GC method for detecting residual quantity of solvent in compound
  • GC method for detecting residual quantity of solvent in compound

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Embodiment Construction

[0018] In the following description, certain specific details are included in order to provide a thorough understanding of the various disclosed embodiments. One skilled in the relevant art will recognize, however, that embodiments may be practiced without one or more of these specific details, and with other methods, components, materials, etc. employed.

[0019] Unless otherwise required in this application, throughout the specification and claims, the word "comprising" shall be interpreted in an open, inclusive sense, ie "including but not limited to".

[0020] References throughout this specification to "an embodiment" or "an embodiment" or "in another embodiment" or "in certain embodiments" mean that in at least one embodiment the Relevant specific reference elements, structures or features described above. Thus, appearances of the phrases "in one embodiment" or "in an embodiment" or "in another embodiment" or "in certain embodiments" in various places throughout the spe...

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Abstract

The invention discloses a method for analyzing a residual quantity of a solvent in a compound by GC (Gas Chromatograph). The method comprises the step of carrying out separation by adopting the following chromatographic conditions: a detector is a hydrogen flame ionization detector, the temperature of the detector is 200 DEG C to 300 DEG C and is preferably 300 DEG C, and the temperature of an injection opening is 180 DEG C to 250 DEG C and is preferably 220 DEG C; a chromatographic column is a medium-polarity capillary gas chromatography column and adopts a programmed temperature process of keeping the temperature of 40 to 60 DEG C for 3 to 10min, then heating to the temperature of 100 to 140 DEG C at a speed of 5 to 15 DEG C/min, keeping the temperature of 100 to 140 DEG C for 1 to 10min, heating to the temperature of 200 to 230 DEG C at a speed of 15 to 25 DEG C/min and keeping the temperature of 200 to 230 DEG C for 1 to 20min; carrier gas is nitrogen, hydrogen or argon and is preferably nitrogen, and the flow rate of the carrier gas is 1ml/min to 10ml/min and is preferably 3ml/min; the solvent is selected from one or more of C1 to C6 carboxylic acid, methanol, ethanol, acetonitrile, ethyl acetate, tetrahydrofuran, methylbenzene and N,N-dimethylformamide; the C1 to C6 carboxylic acid is preferably C1 to C4 carboxylic acid and is more preferably acetic acid. When the method is adopted to detect the residual quantity of the solvent, the operation is simplified, time is saved and cost is saved.

Description

technical field [0001] The present application relates to a method for detecting residual solvent in a compound, in particular to a gas chromatography (GC) method for detecting residual solvent in a compound. Background of the invention [0002] Various solvents are usually used in the synthesis process of compounds such as quinolones, such as acetic acid, methanol, ethanol, acetonitrile, ethyl acetate, tetrahydrofuran, toluene, N,N-dimethylformamide and the like. Among them, acetic acid is difficult to detect due to its high polarity. [0003] Zhang Jianye, Ke Yu, etc. have disclosed the detection of acetic acid using polar capillary chromatographic columns (Zhang Jianye, Ke Yu, Yan Xuebin, Liu Hongmin; Capillary gas chromatography is used to measure ethanol and acetic acid residues in puerarin [J]; Journal of Zhengzhou University (Medical Medicine) ed.); Vol. 40, No. 5, p. 909). [0004] Quinolones work differently from other antimicrobials in that they target the deoxyr...

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 易崇勤兰静郑少辉
Owner NEW FOUNDER HLDG DEV LLC
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