Pretreatment method of ranitidine hydrochloride sample

A technology of ranitidine hydrochloride and sample pretreatment, which is applied in instruments, measuring devices, scientific instruments, etc., can solve the problems of chromatographic column overload and failure to meet the detection limit requirements of NDMA, so as to reduce the technical threshold and avoid degradation into NDMA , the effect of increasing the concentration

Pending Publication Date: 2022-08-02
湖南省药品检验检测研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Measure the HPLC part of N-nitrosodimethylamine in the existing HPLC-MS / MS method ranitidine hydrochloride raw material capsule and tablet and measure, and the chromatographic column is seriously overloaded (need testing solution concentration is 30mg / ml), At the same time can not meet the NDMA detection limit requirements

Method used

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  • Pretreatment method of ranitidine hydrochloride sample
  • Pretreatment method of ranitidine hydrochloride sample
  • Pretreatment method of ranitidine hydrochloride sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0091] Take an appropriate amount of ranitidine or its solid preparation (about 1.5g of ranitidine), add 2.5ml of water precisely, dissolve it by ultrasonic for 2 minutes, precisely add 0.5ml of 0.35g / ml sodium hydroxide solution, shake well, and add 1g of precision 2ml / ml silver nitrate solution, shake well, accurately add 1ml of 0.2g / ml sodium chloride solution, shake well, stand for 10 minutes, centrifuge and filter. The filtrate should be clear and colorless. If it is turbid, it can be frozen at -20°C for 10 minutes, then centrifuged and filtered.

[0092] After repeated verification, under the above proposed operation, ranitidine hydrochloride is almost completely precipitated, and the test solution can change from a pale yellow viscous liquid before precipitation to a clear and non-viscous state. The filtrate of each test batch showed no turbidity after dropwise addition of sodium chloride solution, indicating that the silver ions were completely removed. After more tha...

Embodiment 2

[0110] like Figure 8 As shown, collect the ranitidine hydrochloride capsules of new factory, deal with according to the embodiment of the present invention 1, detect the NDMA lower than the limit, its content determination result is consistent with the current mass spectrometry method detection result, again shows that the inventive method is effective to NDMA. The detection ability reaches the level of mass spectrometry.

Embodiment 3

[0112] Take the same batch of newly manufactured ranitidine hydrochloride capsules and place them at 80°C for 6 hours. Figure 9 As shown, processing according to the present invention results in a detection limit of approximately 1000 times the amount of NDMA. It shows that the method has good specificity and high sensitivity, and also shows that the tendency of ranitidine to degrade in high temperature environment to produce NDMA is very obvious.

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Abstract

The invention discloses a ranitidine hydrochloride sample pretreatment method, which comprises: S1, weighing a ranitidine hydrochloride sample, the ranitidine hydrochloride sample containing an impurity N-nitrosodimethylamine; s2, preparing a ranitidine hydrochloride test solution, and enabling the concentration of N-nitrosodimethylamine in the ranitidine hydrochloride test solution to reach the detection limit of the high performance liquid chromatography; s3, adding an alkaline solution into the ranitidine hydrochloride test solution, and enabling the alkaline solution to completely react with hydrochloric acid in ranitidine hydrochloride to obtain a ranitidine neutralization solution; s4, a silver ion solution is added into the ranitidine neutralization solution, silver ions and secondary amino groups in ranitidine are subjected to a complex reaction completely, and precipitates are generated. According to the method, the ranitidine precipitate in the high-concentration ranitidine test sample is removed, a by-product NDMA is not generated, meanwhile, the NDMA in the sample is reserved, the NDMA detection sensitivity is greatly improved, and the mass spectrum detection requirements of various models are met.

Description

technical field [0001] The invention relates to the treatment of ranitidine hydrochloride samples, in particular to a pretreatment method of ranitidine hydrochloride samples. Background technique [0002] N-nitrosodimethylamine (NDMA) has strong genotoxicity, strong teratogenicity and strong carcinogenicity, and belongs to class 2A carcinogen. The FDA has set a daily intake limit for NDMA of approximately 0.096 μg based on toxicology data in The Carcinogenic Potency Database (CPDB). On September 13, 2019, the FDA issued a safety warning that some ranitidine drugs, which also include the brand-name drug Zantac, contain N-dimethylnitrosamine (NDMA) impurities. Subsequently, my country launched a special inspection and testing of NDMA for this variety. [0003] According to the 2020 edition of the Chinese Pharmacopoeia, the fourth part of the 9306 genotoxic impurity control guidelines, the NDMA content in ranitidine hydrochloride capsules can be deduced according to the compo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/34
CPCG01N30/02G01N30/06G01N30/34G01N2030/027G01N2030/042G01N2030/067
Inventor 李帅廖彬陈鸿玉李钰鑫刘雁鸣唐桂鹏高洋
Owner 湖南省药品检验检测研究院
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