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Method for detecting content of bromopropylene in rocuronium bromide

A technology of rocuronium bromide and propene bromide, applied in the field of analytical chemistry, can solve the problems of human injury, inability to accurately detect the content of propene bromide in rocuronium bromide, etc., and achieve the effects of quality assurance, high sensitivity and strong specificity

Active Publication Date: 2013-04-24
CHENGDU XINJIE HIGH TECH DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, a relatively large amount of propylene bromide is used in the production process of rocuronium bromide, and a molecule of propylene bromide is connected to its structural formula. During the degradation process, the bond may be broken and reduced to produce propylene bromide, and the residue of propylene bromide may cause harm to the human body.
However, there is no detection method for propylene bromide at present, so it is impossible to accurately detect the content of propylene bromide in rocuronium bromide. Therefore, the detection method of propylene bromide content in rocuronium bromide is urgently needed to accurately detect the quality of rocuronium bromide. evaluation to ensure the quality and reliability of the product and the safety of the drug

Method used

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  • Method for detecting content of bromopropylene in rocuronium bromide
  • Method for detecting content of bromopropylene in rocuronium bromide
  • Method for detecting content of bromopropylene in rocuronium bromide

Examples

Experimental program
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Embodiment 1

[0050] Embodiment 1: Determination of the detection wavelength of the detection method of the present invention

[0051] Precisely weigh an appropriate amount of bromopropylene reference substance and prepare a solution containing 20 μg per 1 mL with acetonitrile-water (9:1). According to the ultraviolet spectrophotometry, carry out ultraviolet scanning in the range of 200-400nm. The results are shown in figure 1 .

[0052] Depend on figure 1 It can be seen that allyl bromide has a large absorption only at the end, so 210nm is selected as the detection absorption wavelength.

Embodiment 2

[0053] Embodiment 2: detection method system applicability test of the present invention

[0054] Preparation of the reference substance solution: Accurately weigh 25.12 mg of the propylene bromide reference substance and put it in a 25mL measuring bottle, dissolve it with acetonitrile-water (9:1) and dilute to the mark, shake well; then precisely measure 1 mL and put it in a 100mL measuring bottle, Dissolve and dilute to the mark with acetonitrile-water (9:1), shake well, and use as the reference substance solution.

[0055] Preparation of the test solution: Accurately weigh 104.01mg of rocuronium bromide (081201) and put it in a 10mL measuring bottle, dissolve and dilute to the mark with acetonitrile: water (9: 1), shake well, and make the test solution.

[0056] The detection of propene bromide was carried out mobile phase screening, the results are shown in the following table 1, wherein, with 0.05mol / L tetramethylammonium hydroxide solution of pH5.0 as the aqueous phase o...

Embodiment 3

[0065] Embodiment 3: the selection of detection method solvent of the present invention

[0066] Accurately weighed an appropriate amount of rocuronium bromide samples, respectively with acetonitrile, acetonitrile-water (9: 1), acetonitrile-water (6: 4), water, 0.05mol / L tetramethylammonium hydroxide solution of pH5.0 and Acetonitrile volume ratio is that the mixed solution of 4: 6 is solvent dissolving as need testing solution, gets 5 μ L injection liquid chromatograph respectively, detects under the chromatographic condition described in embodiment 2, record chromatogram, the result is as follows Figure 3-7 .

[0067] Depend on Figure 3-7 Visible, compared with other solvents, when using acetonitrile-water (9: 1) and acetonitrile-water (6: 4) as solvent, the separation degree of rocuronium bromide peak and impurity peak before and after is good, without miscellaneous peak, wherein, When acetonitrile-water (6:4) was used as the solvent, the peak shape of rocuronium bromid...

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Abstract

The invention relates to the field of analytical chemistry and discloses a method for detecting the content of bromopropylene in rocuronium bromide. Particularly, the method comprises the following steps of: taking a rocuronium bromide sample and dissolving the rocuronium bromide sample by using mixed solution with a volume ratio of acetonitrile to water of (9-6):(1-4) as a solvent to obtain tested solution; taking a bromopropylene reference substance and dissolving the bromopropylene reference substance by taking the mixed solution with the volume ratio of acetonitrile to water of (9-6):(1-4) as the solvent to obtain reference substance solution; respectively carrying out high-efficiency liquid chromatography detection on the reference substance solution and the tested solution; and analysing a measuring result by an external standard method. The method for detecting the content of the bromopropylene in the rocuronium bromide can be used for detecting the content of the bromopropylene in a rocuronium bromide product and has the limit of detection of 0.044ng. Due to the establishment of the method, in the process of preparing the rocuronium bromide, the residual amount of the bromopropylene can be detected. The method has high sensitivity, strong specificity and accurate and reliable results, so that the quality of the rocuronium bromide product is accurately evaluated and thequality of the rocuronium bromide product is ensured.

Description

technical field [0001] The invention relates to the field of analytical chemistry, in particular to a method for detecting the content of propylene bromide in rocuronium bromide. Background technique [0002] Rocuronium bromide, the Chinese name is L-[(2B, 3A, 5A, 16B, 17B)-17-(acetyloxy)-3-hydroxy-2-(4-morpholinyl)androst-16-yl ]-1-propenylpyrrole ammonium bromide, the English name is Rocuronium Bromide, referred to as Roc, and the molecular formula is C 32 h 53 BrN 2 o 4 , the molecular weight is 609.6782, and its chemical structural formula is as follows: [0003] [0004] Rocuronium bromide is currently the fastest-acting non-depolarizing muscle relaxant. It is clinically used to assist general anesthesia, facilitate tracheal intubation, and maintain intraoperative muscle relaxation. Like other non-depolarizing drugs, it competitively binds to the cholinergic receptors on the motor nerve terminal synapse to antagonize the effect of acetylcholine. It is safer than...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 聂忠莉王晓玲欧世荣张勇
Owner CHENGDU XINJIE HIGH TECH DEV CO LTD
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