Extraction and detection method of 2-O-beta-D-glucopyranosyl-L-ascorbic acid from fructus malus toringoides and fructus malus tiansitoria
A detection method and technology of medlaric acid, which are applied in chemical instruments and methods, measuring devices, preparation of sugar derivatives, etc., can solve the problems such as unseen russian medlaric acid, etc., and achieve the effect of good application prospect.
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Embodiment 1
[0066] The preparation of embodiment 1 Russian fruit extract
[0067] Take 700g of Eseguo powder (passed through a No. 4 sieve), ultrasonically extract twice with ten times the amount of pure water, each time for 1 hour, combine the extracts to about 15L, after the extracts stand still, take the supernatant and concentrate to 2L at 50°C , the concentrated solution is filtered with 200-300 mesh silica gel, and then filtered with a 0.45 μm micromembrane as the preparation solution,
[0068] Take the above preparation solution and prepare it by high performance liquid chromatography, using C18 chromatographic column, the detection wavelength is 235nm, using methanol: 0.1% phosphoric acid water = 4:96v / v as the eluent in turn, and the flow rate is 0.5 ~ 1.0ml / min. Elution, take the fraction of 13-20min to get the extract of russa fruit, the purity is greater than 80%, the HPLC detection spectrum is shown in figure 1 , the peak with a retention time of 14.727 is the target peak. ...
Embodiment 2
[0069] The preparation method of wolfberry acid in embodiment 2, Russia color fruit
[0070] The Russian fruit extract that embodiment 1 obtains is used as the sample section;
[0071] Take the above sample section, and use the preparative high performance liquid chromatography (chromatographic column: ultimate XB-ODS, 4.6*250mm, 5 μm; Mobile phase: A-methanol B-0.1% phosphoric acid solution; Detection wavelength: UV-235nm; Flow rate: 1.0 mL / min; column temperature: 30°C; see the following table for gradient elution procedure See the detection map figure 2 .
[0072] Table 1. Gradient elution program
[0073] time (min) Mobile phase A(%) Mobile phase B(%) 0~15 1 99 15~25 1→10 99→90 25~30 10→5 90→95 30~40 5 95 40~50 5→1 95→99
[0074] The DAD scan of the target peak is shown in image 3 , see mass spectrometric identification Figure 4 , Figure 5 , see NMR Image 6 , Figure 7 , Figure 8 , Figure 9 , Figure 10 . ...
Embodiment 3
[0084] Embodiment 3, the HPLC content determination of lycitric acid in Russian fruit extract and Russian fruit
[0085] 1. Drugs
[0086] Seventeen batches of Russian fruits were collected, all of which were collected from Luhuo County, Ganzi Prefecture, Sichuan Province. They were identified as Malus toringoides (Rehd.) Hughes and Malus transitoria (Batal. ) Dried ripe fruit of Schneid.
[0087] According to Example 1, 5 batches of russian fruit extract were prepared.
[0088] 2. Reagents and drugs
[0089] Pure water; Methanol (chromatographically pure); Acetonitrile (chromatographically pure); Phosphoric acid (analytical pure);
[0090] 3. Experimental equipment
[0091] KH-500V ultrasonic cleaner; Agilent technologies 1200 high performance liquid chromatography (Agilent Technologies Co., Ltd., USA); SQP electronic analytical balance (Sartorius Scientific Instruments Co., Ltd.).
[0092] 3. Detection method
[0093] 1) Preparation of reference substance
[0094] Acc...
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