Rice syrup extractive and application thereof
A rice syrup and extract technology, applied in sugar derivatives, measuring devices, instruments, etc., can solve problems such as difficult detection of honey, and achieve the effect of simple operation, high accuracy rate, and true and reliable detection results
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Embodiment 1
[0028] Weigh 1000g of rice syrup, add 500ml of water to dissolve, and purify the syrup solution in batches through OASIS HLB (6ml, 500mg) column, each time 30ml of OASIS HLB sample solution, after the sample solution flows out, wash with 3ml of 20% acetonitrile aqueous solution All the eluents were combined, concentrated at 60°C to a viscous liquid, and then dissolved in 50ml of water.
[0029] Adopt preparative liquid chromatography, chromatographic column Zorbax SB-C18, 21.2 * 250mm, mobile phase is 98% water+2% acetonitrile (V / V), flow velocity 15ml / min, injection volume 10ml, detection wavelength 280nm, collect The component after 7.5-10.5 minutes is the target substance. Freeze-dry the collected liquid to obtain a freeze-dried product. According to the concentration of general raw materials, 1 kg of rice syrup can obtain about 4 mg of this substance. The infrared and ultraviolet spectra of the substance are shown in Figure 1a and 1b shown.
[0030] 1 H NMR (400MHz, DM...
Embodiment 2
[0033] Sample source:
[0034] 150 real honey samples from the Bee Product Quality Supervision, Inspection and Testing Center of the Ministry of Agriculture, all of which come from contracted bee factories, and are identified by electronic traceability technology, which can prove that these samples are pure honey. 6 parts of suspected rice syrup adulterated honey: Take 6 parts of real honey, and then take 4 parts of it to be mixed with rice syrup to form honey containing 5% rice syrup by weight, and use the same container to make it indistinguishable in appearance. 32 parts of rice syrup samples come from different provinces and cities of rice syrup production plants, arbitrarily get 1 part of rice syrup in 32 parts of rice syrup samples, and get a small amount of real honey samples to be configured into honey containing 5% rice syrup by weight.
[0035] Analyze with liquid chromatography, use rice syrup extract (formula I) as the target substance to identify these samples, de...
Embodiment 3
[0047] The 21 raw honey samples submitted by a honey company were required to be tested for rice syrup. Using the method of the present invention, using the rice syrup extract POLY-S as the target substance, tandem mass spectrometry is used to confirm whether the samples to be tested are mixed with rice syrup.
[0048] (1) Sample processing:
[0049] Weigh 10g sample, dissolve it with 15mL deionized water, transfer the solution to OASISHLB (200mg, 6mL) small column, activate the small column extraction with 5ml methanol and 10ml water in advance, when the sample liquid flows out, use 3ml 20% acetonitrile Aqueous solution was used for elution, and the eluate was filtered through a filter membrane, and the filtrate was to be determined.
[0050] (2) Liquid chromatography tandem mass spectrometry conditions:
[0051] Agilent 6460 tandem mass spectrometer, column Agilent AQ C18, 2.1×100, 3.5um; column temperature: 30°C; mobile phase: acetonitrile + water (volume ratio), gradient...
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