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Detection method of related substances in aclatonium napadisilate raw materials or preparations thereof

A technology for choline ammonium naphthalate and a detection method, which is applied in the directions of measurement device, material separation, and material analysis, can solve problems such as method specificity and sensitivity that cannot meet quality control, and achieve consistent response, stable baseline, and universality. good effect

Active Publication Date: 2018-06-19
YANGTZE RIVER PHARM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, the relevant literature on the analysis method of naphthalene disulfide ethyl lactoammonium raw material or its preparation is only the dissolution analysis method recorded in the Japanese Orange Book. This method uses an ultraviolet detector for detection and does not involve the detection of impurities. Even in this Optimized on the basis of the method, the specificity and sensitivity of the optimized method still cannot meet the needs of quality control

Method used

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  • Detection method of related substances in aclatonium napadisilate raw materials or preparations thereof
  • Detection method of related substances in aclatonium napadisilate raw materials or preparations thereof
  • Detection method of related substances in aclatonium napadisilate raw materials or preparations thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Detection of related substances in three batches of naphthalene disulfonate bulk drug

[0040] Take an appropriate amount of this product, dissolve and dilute it with a diluent (mobile phase A) to make a solution containing about 10mg per 1ml, as the test solution; accurately measure an appropriate amount of the test solution, and dilute it quantitatively with the diluent to make 1ml contains about 10μg of solution as a control solution.

[0041] Use Thermo Fisher UltiMate3000DGLC high performance liquid chromatograph, use octadecylsilane bonded silica as filler (Waters Atalantis T3, 4.6×250mm, 5μm), column temperature is 25℃; flow rate is 1.0ml / min; detector It is a charged aerosol detector with a temperature of 50℃;

[0042] For related substances, use 0.1% pentafluoropropionic acid aqueous solution as mobile phase A and methanol as mobile phase B. Gradient elution is performed according to the following table, and reverse gradient post-column compensation is performed:

[0...

Embodiment 2

[0049] Detection of related substances in two batches of naphthalene disulfonate capsules

[0050] Take an appropriate amount of this product, dissolve and dilute it with a diluent (mobile phase A) to make a solution containing about 10mg of ethidium naphthalene disulfonate per 1ml, as the test solution; accurately measure the appropriate amount of the test solution, use The diluent was diluted quantitatively to prepare a solution containing approximately 50 μg of ethidium naphthalene per 1 ml as a control solution.

[0051] Use Thermo Fisher UltiMate3000DGLC high performance liquid chromatograph, use octadecylsilane bonded silica as filler (Waters Atalantis T3, 4.6×250mm, 5μm), column temperature is 25℃; flow rate is 1.0ml / min; detector It is a charged aerosol detector with a temperature of 50℃;

[0052] For related substances, use 0.1% pentafluoropropionic acid aqueous solution as mobile phase A and methanol as mobile phase B. Gradient elution is performed according to the followi...

Embodiment 3

[0058] Methodological verification of chromatographic method:

[0059] 1. The positioning test of the raw materials and related substances in the capsules

[0060] According to the methods of Example 1 and Example 2, the raw materials and capsules of naphthalene disulfonate and the related substance reference solution, the raw materials and capsules of naphthalene disulfonate and the mixed solutions of related substances were respectively prepared Liquid chromatograph, record the chromatogram. See the table below for the separation results of the peak of the active ingredient ethyl lactochylammonium and the impurities, and the spectrum figure 2 :

[0061]

[0062] The results show that the ethyl lactocholamine peak in the raw material or its capsules of the ethyl lactocholamine naphthalene disulfonate can be well separated from the related substances and the related substances.

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Abstract

The invention discloses a detection method of related substances in aclatonium napadisilate raw materials or preparations thereof. The method comprises following steps: a reversed-phase high-performance liquid chromatography adopting a countergradient column post-compensation mode is adopted, octadecylsilane chemically bonded silica is taken as a packing material for a chromatographic column, a CAD (charged aerosol detector) is adopted, and a flow phase of a reagent is eluted with volatile negative ions. The detection method has high specificity and sensitivity, has higher precision and accuracy and good durability, is applicable to inspection and quality control of related substances in the aclatonium napadisilate raw materials or preparations thereof, can accurately reflect the content of the related substances in aclatonium napadisilate raw materials or preparations thereof and provides a reasonable basis for formulation of quality standards, so that the quality of products is better controlled and mastered, and the safety of clinical medication is improved.

Description

Technical field [0001] The invention belongs to the technical field of drug analysis, and specifically relates to a method for detecting a raw material of naphthalene disulfonate or its preparation related substances. Background technique [0002] Gastric motility drugs have been used clinically for more than 40 years. Metoclopramide (metoclopramide) came out in the 1960s. It has the effect of promoting gastrointestinal motility and antiemetic, and the effect is definite, but metoclopramide can cause extrapyramidal Department of adverse reactions. Later dopamine is a peripheral dopamine receptor antagonist, characterized by less side effects in the central nervous system, and its limitations are pharmacological effects and narrow treatment ranges, and side effects that cause increased levels of prolactin. At the same time, due to the first pass Effect, oral bioavailability is low. Cisapride, which was listed by Janssen in the 1980s, is a toluamide derivative. Its action site is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/89
CPCG01N30/89
Inventor 杨书明徐镜人蔡伟陈凤琴张雪瑜栾芳刘景龙李浩冬
Owner YANGTZE RIVER PHARM GRP CO LTD
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