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High performance liquid chromatography analysis method and application of benzylnicotinic acid hum salt

A technology of benzylnicotinic acid hum salt and high performance liquid chromatography, which is applied in the field of high performance liquid chromatography analysis of benzyl nicotinic acid humic acid salt, can solve the problem that the detection of impurities in products cannot be controlled, the impurities cannot be analyzed, and the impurities cannot be separated out. Impurities and other problems, to achieve the effect of small precision, simple and easy operation, and high accuracy

Active Publication Date: 2019-05-10
湖北吉和昌化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, in the prior art, there are few articles and reports on the content detection method of BPC-48, and there is no relevant standard release
If only a simple titration method is used, the deviation of the test results will be large, and although the simple ultraviolet spectrophotometer method can detect its content, it cannot separate out impurities, analyze impurities, and cannot detect impurities in central control products. situation detection

Method used

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  • High performance liquid chromatography analysis method and application of benzylnicotinic acid hum salt
  • High performance liquid chromatography analysis method and application of benzylnicotinic acid hum salt
  • High performance liquid chromatography analysis method and application of benzylnicotinic acid hum salt

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Embodiment 1

[0121] 1. Determination of benzyl nicotinic acid salt

[0122] 1.1 Chromatographic conditions of high performance liquid chromatography:

[0123] Column: XB-C18, 5μ, 250mm×4.6mm (with XB-C18 guard column);

[0124] Mobile phase composition volume ratio: acetonitrile: buffer = 10: 90; the buffer solution is 0.013mol / L ammonium acetate solution;

[0125] Flow rate: 0.85mL / min;

[0126] Column temperature: 30°C;

[0127] Detector: UV detector; detection wavelength: 265nm;

[0128] The injection volume is 20 μL.

[0129] 1.2 The method for the determination of benzyl nicotinic acid salt by high performance liquid chromatography comprises the following steps:

[0130] Buffer solution and mobile phase preparation: Accurately weigh 1g of ammonium acetate and dissolve it in a 50mL beaker, transfer it to a 1000mL volumetric flask and dilute it with water, filter it with a 0.45μm aqueous membrane to make a buffer for use; take a 0.45μm organic membrane The filtered acetonitrile...

Embodiment 2

[0172] 1. Determination of benzyl nicotinic acid salt

[0173] 1.1 Chromatographic conditions of high performance liquid chromatography:

[0174] Chromatographic column: Kromasil C18, 5μ, 250mm×4.6mm (with Kromasil guard column);

[0175] Mobile phase composition volume ratio: methanol: buffer = 20: 80; the buffer solution is 0.013mol / L ammonium acetate solution;

[0176] Flow rate: 0.85mL / min;

[0177] Column temperature: 30°C;

[0178] Detector: UV detector; detection wavelength: 265nm;

[0179] The injection volume is 20 μL.

[0180] 1.2 The method for the determination of benzyl nicotinic acid salt by high performance liquid chromatography comprises the following steps:

[0181] Buffer solution and mobile phase preparation: Accurately weigh 1g of ammonium acetate and dissolve it in a 50mL beaker, transfer it to a 1000mL volumetric flask and dilute it with water, filter it with a 0.45μm aqueous membrane to make a buffer for use; take a 0.45μm organic membrane The filt...

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Abstract

The invention discloses a high performance liquid chromatographic analysis method of benzyl pyridinium 3-carboxylate, and application of the high performance liquid chromatographic analysis method. The method comprises the following steps: (a) providing a benzyl pyridinium 3-carboxylate reference solution and a solution of a sample to be tested; (b) analyzing the content of the benzyl pyridinium 3-carboxylate in the solution of the sample to be tested in the step (a) by using high performance liquid chromatography-ultraviolet (HPLC-UV) according to an external standard method, wherein the detection conditions are as follows: a chromatographic column takes octadecyl silane bonded silica gel as filler, a mobile phase is prepared from an organic phase and an acetic acid-ammonia water buffer solution, the organic phase is methyl alcohol or acetonitrile, the volume ratio of the organic phase to the acetic acid-ammonia water buffer solution is equal to (0 to 100)-(80 to 20), and the detection wavelength of an ultraviolet detector is 190-330nm. The high performance liquid chromatographic analysis method solves the technical problems that the method for measuring the content of the benzyl pyridinium 3-carboxylate in the prior art is not perfect and not accurate in results, and can not separate out impurities. The method provided by the invention not only can accurately detect the content of the benzyl pyridinium 3-carboxylate and is good in accuracy, but also can effectively separate out an impurity peak, thus realizing the quality control for the production process of the benzyl pyridinium 3-carboxylate.

Description

technical field [0001] The present invention relates to the technical field of analysis methods for benzyl nicotinic acid salts, in particular, to a high-performance liquid chromatography analysis method and application of benzyl nicotinic acid salts. Background technique [0002] Benzylpyridinium 3-carboxylate (BPC-48) is mainly used in electroplating and galvanizing, as a galvanizing intermediate, and is the main additive in galvanizing additives, which can refine the crystallization of the coating and effectively increase the current density. In the whole acid zinc brightener market, this product is in great demand and has excellent application effect. [0003] The production of BPC-48 is obtained by the reaction of benzyl chloride, nicotinic acid and sodium hydroxide. During the reaction process, there will be unreacted nicotinic acid, benzyl alcohol of raw material benzyl chloride hydrolyzate and by-products of benzyl chloride. Although the unreacted nicotinic acid do...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 何小凤周世骏杨威黄开伟宋文华
Owner 湖北吉和昌化工科技有限公司
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