Method for measuring trace chloridion and sulfate radical in loprazolam samples by ion chromatography

A technology of methanesulfonic acid and ion chromatography, applied in the field of analytical chemistry, to meet the detection requirements, high accuracy, and easy to operate

Active Publication Date: 2013-02-06
ANHUI WAYEE SCI & TECH CO LTD
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  • Abstract
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  • Claims
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Problems solved by technology

[0003] The object of the present invention is to solve the problem of the determination of trace chloride ion and sulfate radical content in the methanesulf...

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  • Method for measuring trace chloridion and sulfate radical in loprazolam samples by ion chromatography
  • Method for measuring trace chloridion and sulfate radical in loprazolam samples by ion chromatography
  • Method for measuring trace chloridion and sulfate radical in loprazolam samples by ion chromatography

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Embodiment

[0042] (1) Reagent preparation:

[0043] Eluent: Accurately weigh 0.2544g of sodium carbonate reference reagent, dilute 1000 times with deionized water,

[0044] Obtain the eluent of 2.4mmol / L; Accurately weigh 0.3816g sodium carbonate reference reagent, dilute 1000 times with deionized water, obtain the eluent of 3.6mmol / L; Accurately weigh 0.5088g sodium carbonate reference reagent, use two Diluted 1000 times with deionized water to obtain 4.8mmol / L eluent;

[0045] Select the sodium carbonate solution of 2.4, 3.6 and 4.8mmol / L respectively as eluting solution, carry out to actual sample

[0046] Measure, under the chromatographic condition of 4.8mmol / L sodium carbonate, the degree of separation of methanesulfonic acid and chloride ion is less than 1.5, does not reach baseline separation, affects the accurate quantification of chloride ion in the actual sample; And adopt 2.4mmol / L sodium carbonate as Eluent, the separation degree of methanesulfonic acid and chloride ion ca...

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Abstract

The invention discloses a method for measuring trace chloridion and sulfate radical in loprazolam samples by ion chromatography and belongs to the field of analytic chemistry. The method includes the followings steps of preparing and analyzing Cl- and SO42- mixed standard solution and obtaining a linear equation of concentration and peak area, pretreating the loprazolam samples, feeding the treated loprazolam samples to an ion chromatography by a disposable needle type filter, utilizing 3.6mmol/L sodium carbonate as leacheate and analyzing and measuring the content of the chlorodion and the sulfate radical according to the obtained linear equation, wherein a chromatographic column adopted in the ion chromatography is a high-capacity chromatographic column, the inner diameter of filler of the chromatographic column is 5 micrometers, the temperature of a column temperature box is set to be 45 DEG C, sampling input quantity is 100 microliters, applied curb current is 40mA, and flow velocity is 0.8ml/min. The method is quick and simple, high in accuracy, convenient and easy to operate and applicable to quality control in the process of production of loprazolam, the integral analyzing process can be completed within 25min, and the detection requirements of the fine chemical industry are met.

Description

technical field [0001] The invention relates to a method for quantitatively measuring the contents of chloride ions and sulfate radicals in high-purity methanesulfonic acid samples, in particular to a method for determining the contents of trace chloride ions and sulfate radicals in methanesulfonic acid samples by ion chromatography. belongs to the field of analytical chemistry. Background technique [0002] Methanesulfonic acid is usually used as a raw material in the production of medicines and pesticides, and it can also be used as a dehydrating agent, a coating curing accelerator, a fiber treatment agent, a solvent, and a catalyst for racination, esterification, and polymerization. The presence of impurity ions, chloride ions and sulfate radicals in methanesulfonic acid reagents will have an impact on product performance and equipment safety, and sulfuric acid and chlorine-containing substances will be used in the production of methanesulfonic acid, so there must be chlo...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 焦霞
Owner ANHUI WAYEE SCI & TECH CO LTD
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