Method for determining glucose and gluconic acid in oxidized dextrin
A determination method and a technology for oxidative dextrin, applied in the field of medicine, can solve the problems of low sensitivity, inappropriate peak time, indeterminate gluconic acid content, etc., and achieve the effect of high sensitivity
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Embodiment 1
[0040] Preparation of sample solution:
[0041] (1) Weigh 0.1g of the oxidized dextrin sample, add 1ml of sulfuric acid with a mass percentage of 10%, destroy it in an oil bath at 100°C for 1h, and dilute to 10ml with water after cooling;
[0042] (2) Measure 0.2 ml of the solution obtained in step (1), dilute to 100 ml with water, mix well, pass through a 0.22 micron water film as the sample solution.
[0043] Preparation of mobile phase solution:
[0044] (1) Preparation of 200mmol / L NaOH solution: Measure 16ml of NaOH solution with a mass percentage of 50% into a beaker, add 1000ml of water, stir evenly, pass through a 0.22 micron water film, and put it into the mobile phase bottle;
[0045] (2) Preparation of 500mmol / L NaOAc solution: Weigh 41g NaOAc into a beaker filled with 10001ml water, stir to dissolve, pass through a 0.22 micron water film into the mobile phase bottle.
[0046] Preparation of standard curve solution:
[0047] (1) Weigh 20mg of glucose and 5.2mg of...
Embodiment 2
[0051] Ion chromatography instrument selection and parameter setting:
[0052] Instrument model: Thermo-Fisher ICS-5000+
[0053] Guard column name: Dionex CarboPacTM PA20 BioLCTM 3*30mm Guard
[0054] Analytical column name: Dionex CarboPacTM PA20 BioLCTM 3*150mm Analytical
[0055] Column temperature: 30°C
[0056] Electrochemical detector parameter setting:
[0057] Amperometric Parameters (Amperometric Detector) Electrode Material: Gold Electrode
[0058] Reference electrode: Ag / AgCl
[0059] Potential waveform: sugar four potential waveform
[0060] Detector temperature: 28~32℃
[0061] with mobile phase H 2 O, mobile phase NaOH solution (200mmol / L) and mobile phase NaOAc solution (500mmol / L) carry out gradient elution as eluent, and elution condition is as shown in table 1, then setting flow velocity is 0.4ml / min, carries out The sample volume was 5 μL, and the sample was injected for analysis.
[0062] Table 1
[0063] time (min) h 2 O(%)
Embodiment 3
[0065] The standard curve solution prepared in Example 1 was injected with an injection volume of 5 μL, and a standard curve was drawn. The correlation coefficients of the standard curve are shown in Table 2.
[0066] Table 2
[0067] Peak Name Cal. Type linear correlation coefficient intercept slope Linear range (mg / L) glucose LOff 0.9998 1.7420 2.8074 4~20 gluconic acid LOff 0.9999 0.0008 0.3987 1~5
[0068] Then, the sample solution prepared in Example 1 was injected, and the injection volume was 5 μL. After calculation, the contents of glucose and gluconic acid in the sample solution were shown in Table 3.
[0069] table 3
[0070]
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