Sample pretreatment method for simultaneous determination of oxalic acid, succinic acid, sulfuric acid and phosphate radicals in regenerated tobacco leaves through ion chromatography
A technology for sample pretreatment and reconstituted tobacco leaves, which is applied to measurement devices, material separation, instruments, etc., and can solve the problems of incomplete extraction of oxalic acid, failure to consider the influence of vitamin C, and inaccurate measurement results.
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Embodiment 1
[0038] Example 1 The impact experiment of vitamin C on the determination of oxalic acid
[0039] 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
[0040] The research experiment of embodiment 2 sample pretreatment method
[0041] 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
[0044] The determination experiment of embodiment 3 chromatographic conditions
[0045] 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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