Method for simultaneously detecting 26 organic acids and inorganic negative ions in juice
A technology of inorganic anions and organic acids, applied in the field of chemistry, can solve the problems of inability to meet the requirements of simultaneous detection, failure to meet detection requirements, and low detection efficiency, and achieve reduced detection costs, less matrix interference components, and high detection sensitivity Effect
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[0039] Example one
[0040] Determination of chromatographic conditions
[0041] 1. Chromatographic column selection: The experimental separation effects of AS11, AS11-HC, and AS19 columns were successively investigated, and it was found that under the same conditions, the AS11-HC column has the sharpest peak shape and the best comprehensive separation effect. This is because AS11-HC is a high-capacity chromatographic column, which has good retention of organic acids and inorganic anions, and is very suitable for simultaneous detection of multiple components. Therefore, the AS11-HC column was selected for experimental determination.
[0042] 2. Selection of flow rate: the experimental separation under flow rate conditions of 0.5mL / min, 1.0mL / min, 1.5mL / min, and 2.0mL / min have been investigated successively, and the chromatographic separation effect at 0.5mL / min is better than 1.0mL / min Although the resolution is slightly larger than that at 1.0 mL / min, the total peak time becomes l...
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[0046] Example two
[0047] The accuracy of the measurement method
[0048] 1. Detection limit and calibration curve
[0049] Prepare standard working solutions of 18 kinds of organic acids and 8 kinds of inorganic anions with different concentrations respectively, and test on the computer to obtain chromatographic separation diagrams of 26 kinds of standard solutions, see the attached drawings in the instructions for details figure 1 . The detection limit (S / N=3) of the component to be tested is calculated by the chromatographic peak signal-to-noise ratio. In the concentration range of 0.02mg / L to 10.0mg / L, 9 different concentration points (0.02, 0.04, 0.10, 0.20, 0.50, 1.0, 2.0, 5.0, 10.0mg / L) standard working solution detection and linearity The fitting and correlation coefficients are both greater than 0.995, indicating that under the experimental conditions, the linearity is good when multiple components are detected simultaneously. See Table 2 for details, where Y is the pea...
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[0073] Example three
[0074] Actual sample measurement
[0075] Six common fruit juice drinks (apple juice, grape juice, orange juice, peach juice, pear juice, mixed juice) were selected, and the contents of organic acids and inorganic anions in actual samples were detected.
[0076] Before the test, use a KOH solution with a concentration of 4.0mol / L, adjust the pH to neutral (6.5-8.0), take 10mL of the sample into a 50mL centrifuge tube, centrifuge at a high speed at 10000r / min for 15min, and weigh the supernatant The sample is 1.00g, dilute to a 100mL volumetric flask with ultrapure water. Shake well, let it stand for 10 minutes, take 10.0 mL of the solution, pass through a 0.22 μm water phase filter membrane, discard the first 3 mL, collect the clear liquid afterwards, and wait for testing.
[0077] The resulting supernatant was tested on the machine according to ion chromatography conditions and multi-stage gradient elution procedures, and the results were calculated.
[0078] T...
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