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Method for determining content of acrolein in nitroglycerin solution by UPLC-MS/MS

A technology of nitroglycerin and acrolein, used in measuring devices, instruments, scientific instruments, etc.

Pending Publication Date: 2021-05-18
上海微谱检测科技集团股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the nitroglycerin solution will be hydrolyzed to produce acrolein under alkaline conditions. In the actual production and transportation, the nitroglycerin solution cannot avoid the impurity of acrolein. The presence of acrolein has a pungent smell, and its existence will also affect nitric acid. The use effect of glycerin solution, therefore, the whole process of effective detection of nitroglycerin solution production and transportation has become an urgent research topic that enterprises must solve

Method used

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  • Method for determining content of acrolein in nitroglycerin solution by UPLC-MS/MS
  • Method for determining content of acrolein in nitroglycerin solution by UPLC-MS/MS
  • Method for determining content of acrolein in nitroglycerin solution by UPLC-MS/MS

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Effect test

Embodiment 1

[0129] Embodiment 1 of the present invention specifically provides a method for determining the content of acrolein in nitroglycerin solution by UPLC-MS / MS, the steps comprising:

[0130] 1. Solution preparation

[0131] 1.1 Diluent, formic acid-purified water (0.1:100), measure 500ml of purified water into a 500ml solvent bottle, add 500.0μl of formic acid, shake well, degas by ultrasonic for 10min, record as A;

[0132] 1.2 Derivatization solution, weigh 120 mg of 2,4-dinitrophenylhydrazine, add 200 ml of acetonitrile to dissolve, oscillate and shake well, degas it by ultrasonic for 10 min, record it as B;

[0133] 1.3 Mobile phase, mobile phase A: formic acid-methanol (0.1:100), measure 500ml of methanol into a 500ml solvent bottle, add 500.0μl of formic acid, shake well, degas by ultrasonic for 10min; mobile phase B: formic acid-purified water ( 0.1:100), measure 500ml of purified water into a 500ml solvent bottle, add 500.0μl of formic acid, shake well, and degas by ultr...

Embodiment 2

[0149] Example 2 of the invention provides a method for determining the content of acrolein in nitroglycerin solution by UPLC-MS / MS. The specific implementation method is the same as that of Example 1, except that the column temperature in the instrument method is 45°C.

[0150] The final test results show that the selectivity is reduced, which is not conducive to separation.

Embodiment 3

[0152] Embodiment 3 of the invention provides a method for determining the content of acrolein in nitroglycerin solution by UPLC-MS / MS. The specific implementation method is the same as that of Embodiment 1, except that the flow rate in the instrument method is 0.6 mL / min.

[0153] The final test results show that the acrolein target peak is difficult to distinguish from the impurity peak.

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Abstract

The invention relates to a method for detecting impurities in a nitroglycerin solution, and particularly relates to a method for determining a content of acrolein in a nitroglycerin solution by UPLC-MS / MS. The method for determining the content of acrolein in the nitroglycerin solution by UPLC-MS / MS comprises the following steps: adding a derivatization solution into a nitroglycerin sample solution, diluting with a diluent, uniformly mixing by vortex, reacting at 50-100 DEG C for 1-5 hours, taking out to obtain a pretreatment solution, and carrying out UPLC-MS / MS analysis; and calculating the content of the acrolein in the nitroglycerin sample solution based on a standard working curve and a regression equation obtained by testing the standard working solution under the same condition. The method for determining the content of acrolein in the nitroglycerin solution through UPLC-MS / MS provided by the invention has a very good separation effect, the symmetry of characteristic peaks corresponding to target components in a test spectrogram is good, and the characteristic peaks corresponding to the target components are not influenced by impurity peaks. And the detection method provided by the invention has good accuracy and repeatability.

Description

technical field [0001] The invention relates to a method for detecting impurities in nitroglycerin solution, in particular to a method for determining the content of acrolein in nitroglycerin solution by UPLC-MS / MS. Background technique [0002] Nitroglycerin solution is mainly produced by the reaction of glycerol and nitrate esters. It can relax vascular smooth muscle, dilate veins and coronary arteries, and has the characteristics of fast absorption and rapid onset of action. It can be used for the treatment and prevention of angina pectoris in coronary heart disease. It is also used to lower blood pressure or treat congestive heart failure. However, the nitroglycerin solution will be hydrolyzed to produce acrolein under alkaline conditions. In the actual production and transportation, the nitroglycerin solution cannot avoid the impurity of acrolein. The presence of acrolein has a pungent smell, and its existence will also affect nitric acid. The use effect of glycerin so...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/72G01N30/06G01N30/86G01N30/88
CPCG01N30/02G01N30/72G01N30/06G01N30/8634G01N30/88G01N2030/067G01N2030/8872G01N2030/884
Inventor 李美玲秦秋明付佳佳刘建丽
Owner 上海微谱检测科技集团股份有限公司
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