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A kind of assay method for detecting trace hydroxylamine hydrochloride in medicine

A hydroxylamine hydrochloride and determination method technology, applied in the field of analytical chemistry, can solve the problems of low sensitivity, measurement interference, complicated operation, etc., and achieve the effects of good reproducibility, small sampling volume and simple operation

Active Publication Date: 2015-11-18
江苏省药物研究所有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As for the determination of hydroxylamine hydrochloride, currently there are redox titration, acid-base titration and spectrophotometry, etc., the above methods all need to carry out derivatization reaction to hydroxylamine hydrochloride to indirectly measure the content of hydroxylamine hydrochloride, the operation is complicated, and the related coexisting ions are easy to detect. The measurement produces interference, and its sensitivity is low, and the sampling volume is large

Method used

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  • A kind of assay method for detecting trace hydroxylamine hydrochloride in medicine
  • A kind of assay method for detecting trace hydroxylamine hydrochloride in medicine
  • A kind of assay method for detecting trace hydroxylamine hydrochloride in medicine

Examples

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Effect test

Embodiment 1

[0030] An assay method for detecting trace amounts of hydroxylamine hydrochloride in medicine, said assay method comprising the steps of:

[0031] Preparation of the test sample: Take 0.1 g of risperidone and add 4 mL of methanol to dissolve it, dilute it with water to a solution containing 10 mg per 1 mL, filter it through an activated C18 solid-phase extraction column, and obtain it.

[0032] Preparation of the reference substance stock solution: Take an appropriate amount of hydroxylamine hydrochloride, dissolve it with 40% methanol and dilute it into a solution of hydroxylamine hydrochloride containing 10 ppm per 1 mL.

[0033] Preparation of the reference substance solution: draw 2.5mL of the reference substance stock solution into a 50mL measuring bottle, dissolve and dilute it into a hydroxylamine hydrochloride reference substance solution containing 0.5ppm per 1mL with 40% methanol.

[0034] Preparation of risperidone solution of 0.5ppm hydroxylamine hydrochloride refe...

Embodiment 2

[0041] An assay method for detecting trace amounts of hydroxylamine hydrochloride in medicine, said assay method comprising the steps of:

[0042] Preparation of the test sample: take 0.1 g of hydroxyurea, dissolve it in water, dilute it with water to a solution containing 10 mg per 1 mL, filter it through an activated C18 solid-phase extraction column, and obtain it.

[0043] Preparation of reference substance stock solution: Take an appropriate amount of hydroxylamine hydrochloride, dissolve it in water and dilute it into a solution of hydroxylamine hydrochloride containing 10 ppm per 1 mL.

[0044] Ion chromatography, using post-column rehydration derivation method, using CS16 cation exchange chromatography column (0.5×250mm); eluent is 35mmol / L methanesulfonic acid solution, flow rate is 1.2mL / min, post-column rehydration is 500mmol / L potassium hydroxide solution, the flow rate is 0.2mL / min. The detector is an amperometric detector, Au is used as the electrode, Ag-AgCl e...

Embodiment 3

[0049] An assay method for detecting trace amounts of hydroxylamine hydrochloride in medicine, said assay method comprising the steps of:

[0050] Preparation of the test sample: take roxithromycin 0.1g and add 5mL ethanol to dissolve it, dilute it with water to a solution containing 10mg per 1mL and filter it through an activated C18 solid phase extraction column to obtain

[0051] Preparation of reference substance stock solution: Take an appropriate amount of hydroxylamine hydrochloride, add 50% ethanol to dissolve and dilute it into a solution of hydroxylamine hydrochloride containing 10ppm per 1mL.

[0052]Ion chromatography, using post-column rehydration derivation method, using CS16 cation exchange chromatography column (0.5×250mm); eluent is 25mmol / L methanesulfonic acid solution, flow rate is 0.8mL / min, post-column rehydration is 200mmol / L L potassium hydroxide solution, the flow rate is 0.5mL / min. The detector is an amperometric detector, Au is used as the electrode...

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Abstract

The invention discloses a method for detecting trace amounts of hydroxylamine hydrochloride in medicines. The sample treatment of the invention is to take a certain amount of medicines, dissolve them in water or an organic solvent, and filter them through an activated C18 solid-phase extraction column, and take the subsequent filtrate as a test product solution. The analysis method adopts ion chromatography, adopts post-column rehydration derivation method, uses CS16 cation exchange chromatography column, eluent is methanesulfonic acid solution, and post-column rehydration is sodium hydroxide or potassium hydroxide solution. The main advantages of the present invention are: 1) This method does not require derivatization of hydroxylamine hydrochloride, and adopts a direct measurement method, which is simple to operate and effectively avoids interference; 2) The pre-treatment of the sample is filtered by a C18 solid-phase extraction column, which can effectively remove Relevant organic substances can reduce the damage to the cation exchange chromatography column and the interference to the determination; 3) The sample volume is small, the detection sensitivity is increased by an order of magnitude, and the reproducibility is good.

Description

Technical field [0001] The present invention is an analytical chemistry field, which involves a measurement method for detecting marks in the drug. Background technique [0002] Hydroxyline hydrochloride is mainly used as a reducing agent and analogy. It is used in organic synthesis to prepare crickets. It is also used as raw materials for synthetic anticancer drugs (hydroxylpines), sulfa drugs (New Nuo Ming) and pesticide (extinguishing Dovi).In recent years, it has been used to synthesize antibiotics such as Achicycin, craticin, and loboin. [0003] Hyl Hyl Hyl Hyl Hyl Hyl Hyl Hyl Hyl Hyl Hyl Hyl Hyl Hyl Hylolytic's Frequent toxicity and Genetic mutation effects, detecting its residues in drugs and controlling its limitations is an important aspect of ensuring the safety and effectiveness of drug usage, and ensuring the quality of the drug.Regarding the measurement of hydrochloride hydrochloride, currently the main aerobic reduction method, acid -alkali drip method, and spaghet...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06G01N30/02
Inventor 陈国广苗燕飞欧阳平凯
Owner 江苏省药物研究所有限公司