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Ion chromatography method for simultaneous determination of oxalic ion, succinate ion, sulfate ion and phosphate ion in reconstituted tobacco and application thereof

A technology of reconstituted tobacco leaves and ion chromatography, applied in measuring devices, material separation, instruments, etc., can solve the problems of high measurement results, incomplete extraction of oxalic acid, and no consideration of the influence of vitamin C, etc., to achieve accurate quantitative results of oxalic acid

Active Publication Date: 2016-03-02
CHINA TOBACCO GUANGDONG IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are many ion chromatography methods for the determination of oxalic acid content in plants and foods containing vitamin C (ascorbic acid) including tobacco, but the above literatures do not consider the influence of vitamin C on the determination of oxalic acid, and only consider vitamins in the medical detection of biological fluids. The effect of C on the determination of oxalic acid
There are two problems in the current method for measuring oxalic acid in tobacco: the one is incomplete extraction of oxalic acid with pure water as the extract; Converted to oxalic acid to make the measurement result higher

Method used

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  • Ion chromatography method for simultaneous determination of oxalic ion, succinate ion, sulfate ion and phosphate ion in reconstituted tobacco and application thereof
  • Ion chromatography method for simultaneous determination of oxalic ion, succinate ion, sulfate ion and phosphate ion in reconstituted tobacco and application thereof
  • Ion chromatography method for simultaneous determination of oxalic ion, succinate ion, sulfate ion and phosphate ion in reconstituted tobacco and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1 The impact experiment of vitamin C on the determination of oxalic acid

[0034] At present, many ion chromatography methods for the determination of oxalic acid content in plants containing vitamin C, including tobacco, use NaOH solution as the eluent to separate oxalate and other anions. This study found that vitamin C can be converted to oxalate at high pH. Prepare 100ug / ml vitamin C standard solution with water as solvent, and use 10mmol / L, 20mmol / L, 30mmol / L NaOH solution for isocratic elution and 11mmol / L~50mmol / L NaOH solution gradient elution respectively on AS18 anion analysis column as Mobile phase procedure, measure vitamin C standard solution, all have oxalic acid group to go out peak on test chromatogram (retention time qualitative, see figure 1 shown). figure 2 Shown is the amount of oxalic acid produced when the 100ug / mL vitamin C standard solution prepared under two solvent bases of pure water and methanesulfonic acid is eluted with different...

Embodiment 2

[0035] The research experiment of embodiment 2 sample pretreatment method

[0036] The four target substances to be tested are all water-soluble anions. For ion chromatography detection, the commonly used extraction solvents are pure water, acid solution and sodium hydroxide solution. Due to the reason of 2.1, strong alkaline solution cannot be used for extraction. In the test, pure water was used as the extraction solvent to extract the reconstituted tobacco leaf samples and the residue after the first extraction by shaking for 30 minutes, and four target components were determined. The results show that using pure water as the extractant, the extraction efficiency of oxalic acid is only 37.7%, which cannot be extracted completely at one time. Since the analytical column used in this method is an anion column, commonly used acid ions will cause anion interference, so different concentrations of methanesulfonic acid (MSA) were used as the extraction solvent in the experiment....

Embodiment 3

[0039] The determination experiment of embodiment 3 chromatographic conditions

[0040] Based on the summary of long-term research experiments of the present invention and the aforementioned reasons, NaOH solution cannot be used as the eluent, and the test explores the use of NaCO 3 +NaHCO 3 Possibility as mobile phase, the results show (see Figure 5 ), using 4.5mmol / LNaCO 3 +1.4mmol / LNaHCO 3 As eluent, vitamin C standard solution was not converted into oxalic acid. At the same time, a variety of chromatographic columns were studied and investigated, such as AS14, AS22 and other chromatographic columns, and multiple factors such as resolution, peak shape symmetry, peak width and sensitivity were compared and analyzed, and AS22 was preferably determined as the analytical column of this method. The two target components are well separated on this column; the influence of mobile phase flow rate and injection volume is compared, the flow rate is 1.2ml / min, increasing the inje...

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Abstract

The invention discloses an ion chromatography method for simultaneous determination of oxalic ion, succinate ion, sulfate ion and phosphate ion in reconstituted tobacco The method established in the invention uses methanesulfonic acid as an extraction liquid to guarantee the extraction efficiency of each group to be tested in a sample reach above 99.7%; a mixed solution of sodium carbonate and sodium bicarbonate is used as a mobile phase, in order to effectively eliminate the effects of degradation of vitamin C on the quantification of oxalic acid; sample treatment and sampling at a time can simultaneously detect four components including oxalic ion, succinate ion, sulfate ion and phosphate ion in reconstituted tobacco; and the relative standard deviation of content of each group to be tested is 0.27%-0.99%, the adding standard recovery is 99.3%-106.2%. The method is accurate, simple and reliable, and is applicable to the determination of relative groups in tobacco samples and reconstituted tobacco samples.

Description

technical field [0001] The technical field of detection of reconstituted tobacco leaves of the present invention, more specifically, relates to an ion chromatography detection method and application for simultaneous determination of oxalic acid, succinic acid, sulfuric acid and phosphate in reconstituted tobacco leaves. Background technique [0002] Paper-making reconstituted tobacco has been increasingly used because of its advantages of balancing tobacco structure, stabilizing cigarette quality, and effectively reducing the release of tar and some harmful components. During the processing of reconstituted tobacco leaves by the papermaking method, various auxiliary agents need to be added, wherein succinic acid (succinic acid) and oxalic acid are used as process auxiliary agents, and phosphoric acid is added as an extraction auxiliary agent. Based on the stable quality and safety considerations of reconstituted tobacco products, the addition of various additives should be s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
Inventor 施文庄胡静李峰
Owner CHINA TOBACCO GUANGDONG IND
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