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Method for detecting content of NDMA in tidine drug

A detection method and drug technology, applied in the field of analysis and testing, can solve the problems of high cost, limited applicability of LC-APCI-MS/MS and LC-HRMS, false positive results, etc., and achieve low cost and strong transformation and application prospects , The effect of small mass spectrometry pollution

Active Publication Date: 2020-08-14
HUNAN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Moreover, since APCI is a high-temperature ion source, it will also cause the new NDMA produced by the pyrolysis of the drug itself to overlap with the residual NDMA in the sample, resulting in false positive results. In addition, the HRMS instrument is very expensive, which largely limits the ability of LC- Applicability of APCI-MS / MS and LC-HRMS

Method used

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  • Method for detecting content of NDMA in tidine drug
  • Method for detecting content of NDMA in tidine drug
  • Method for detecting content of NDMA in tidine drug

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] A kind of method of detecting NDMA content from certain batch of nizatidine raw material of the present invention, concrete steps are as follows:

[0053] (1) Weigh 120mg of nizatidine crude drug in a 15mL centrifuge tube, add 4mL of acetonitrile, vortex for 2min, shake for 30min, centrifuge for 5min, pass through a 0.22mm organic membrane to make a sample injection solution;

[0054] (2) The sample liquid is separated by liquid chromatography, and the specific process conditions include:

[0055] Chromatographic column: Waters hydrophilic column: XBridge BEH HILIC (150×2.1mm, 2.5μm);

[0056] Pre-column mobile phase: mobile phase (B) 95% acetonitrile, mobile phase (A): pure water; isocratic elution;

[0057] Column tail mobile phase (C): 10% acetonitrile+200mmol / L formic acid;

[0058] Flow rate: The flow rate ratio of the mobile phase flow rate before the column / the flow rate at the end of the column: 2:1 (0.2mL / min:0.1mL / min);

[0059] Injection volume: 20uL;

[...

Embodiment 2

[0065] A method for detecting NDMA content from a certain batch of nizatidine preparations of the present invention, the specific steps are as follows:

[0066] (1) After crushing the dispersible tablet, weigh 150mg into a 15mL centrifuge tube, add 5mL of acetonitrile, vortex for 2min, shake for 60min, centrifuge for 5min, pass through a 0.22mm organic membrane to make a sample solution;

[0067] (2) The sample liquid is separated by liquid chromatography, and the specific process conditions include:

[0068] Chromatographic column: Waters hydrophilic column: XBridge BEH HILIC (150×2.1mm, 2.5μm);

[0069] Pre-column mobile phase: mobile phase (B): 95% acetonitrile, mobile phase (A): pure water; isocratic elution;

[0070] Mobile phase at the end of the column: 10% acetonitrile + 200mmol / L formic acid;

[0071] Flow rate: The flow rate ratio of mobile phase flow rate before the column / mobile phase flow rate at the end of the column: 2:1 (0.2mL / min:0.1ml / L);

[0072] Injectio...

Embodiment 3

[0076] A method of detecting NDMA content from a certain batch of nizatidine raw material (different batches from Example 1) of the present invention, concrete steps are as follows:

[0077] (1) Weigh 120mg of nizatidine crude drug in a 15mL centrifuge tube, add 4mL of acetonitrile, vortex for 2min, shake for 30min, centrifuge for 5min, pass through a 0.22mm organic membrane to make a sample injection solution;

[0078] (2) The sample liquid is separated by liquid chromatography, and the specific process conditions include:

[0079] Chromatographic column: Waters hydrophilic column: XBridge BEH HILIC (150×2.1mm, 2.5μm);

[0080] Pre-column mobile phase: mobile phase (B): 95% acetonitrile, mobile phase (A): pure water; isocratic elution;

[0081] Column tail mobile phase (C): 10% acetonitrile+200mmol / L formic acid;

[0082] Flow rate: The flow rate ratio of the mobile phase flow rate before the column / the flow rate at the end of the column: 2:1 (0.2mL / min:0.1mlLmin);

[0083...

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Abstract

The invention discloses a method for detecting the content of NDMA in a tidine drug. The method adopting liquid chromatography-mass spectrometry detection comprises the following steps: (1), separating a tidine drug sample by using liquid chromatography that adopts a hydrophilic interaction chromatographic column, and has no acid added into a pre-column mobile phase; and (2), detecting the NDMA content of the sample subjected to liquid chromatography separation in combination with mass spectrometry. According to the invention, a hydrophilic interaction chromatographic analysis method is adopted to separate the tidine component and the NDMA; acid is not added into the pre-column mobile phase, so that the tidine and the NDMA are kept in a non-ionic state to be separated, the separation timedifference between the tidine and the NDMA is 12-13 minutes; and thus the interference of tidine components on the NDMA can be completely removed, and the quantitative result is accurate. According tothe method, electrospray ionization is combined with tandem mass spectrometry, ESI is low-temperature mass spectrometry, the mass spectrometry part is non-high in resolution, and the manufacturing cost is relatively low, so that the application and popularization performance is higher, and the conversion and application prospect is good.

Description

technical field [0001] The invention belongs to the field of analysis and testing, in particular to a method for detecting the content of NDMA in tindins. Background technique [0002] Nizatidine is a drug widely used clinically in the treatment of hyperacid secretion diseases. It is a third-generation novel H2-receptor antagonist. Similar to ranitidine, this type of drug has also been detected to contain Safe levels of the carcinogen NDMA. NDMA, the full name in Chinese is N-nitrosodimethylamine, which has been identified as a genotoxic impurity, which can cause DNA damage in human genetic material at very low concentrations, thereby causing gene mutations and tumorigenesis. At present, the detection methods of NDMA impurities in drug raw materials and preparations issued by FDA, EMA, NMPA and other drug regulatory authorities mainly include: GC-MS (gas chromatography mass spectrometry), LC-APCI-MS / MS (liquid chromatography-atmospheric pressure chemistry ionization tandem...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/72G01N30/86
CPCG01N30/02G01N30/06G01N30/34G01N30/7233G01N30/8679
Inventor 陈波郭萍
Owner HUNAN NORMAL UNIVERSITY
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