Response surface method optimized method for extracting 1-deoxynojirimycin in mulberry leaves with acidic ethanol solution
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A deoxynojirimycin and solution extraction technology, applied in organic chemistry and other fields, can solve the problems of 1-DNJ structure damage, complicated process, and reduced bioavailability
Inactive Publication Date: 2014-04-30
GUANGZHOU GENERAL HOSPITAL OF GUANGZHOU MILITARY COMMAND
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However, the decoction method will destroy the structure of 1-DNJ and reduce its bioavailability; the reflux method and ultrasonic-assisted extraction method have the disadvantages of complicated process and not conducive to large-scale industrial production.
These current extraction methods are difficult to meet people's needs for 1-DNJ
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Embodiment 1
[0035] 1. The standard curve and HPLC-ELSD detection spectrum of 1-DNJ
[0036] 1) Standard curve drawing
[0037] Precisely weigh 3.56mg of 1-DNJ standard substance into a 50mL volumetric flask, and dissolve it in ultrapure water to prepare a content of 71.2μg·mL -1 The sample volumes were 5 μL, 10 μL, 20 μL, 30 μL and 40 μL respectively, and a standard curve was made according to the relationship between mass and peak area. Perform linear regression on the peak area Y- with the standard product 1-DNJ standard solution quality X-, the resulting regression equation is Y=624.56X-112.74, R 2 =0.9991, at 0.356~2.848μg·mT -1 There is a good linear relationship between the mass concentration and the peak area within the range (see figure 1 ).
[0038] 2) Detection spectrum of high performance liquid chromatography evaporative light detector (HPLC-ELSD)
[0039] Use HCl to adjust the pH of the ethanol solution to about 6.5 as the extraction solvent. Accurately weigh 10.0 g of m...
Embodiment 2
[0078] Extraction method of mulberry leaf 1-DNJ optimized by response surface methodology
[0079] 1) Take an ethanol solution with a volume concentration of 66.5%, and use HCl to adjust the pH value to 6.7 as an extraction solvent, add 10g of mulberry leaf powder, and make the liquid-to-material ratio 25, that is, 25ml extraction solvent / g mulberry leaf coarse powder, place in Extract in a constant temperature water bath at 80°C for 2.7 hours, and filter with suction to obtain the preliminary extract of 1-DNJ and the filter residue of mulberry leaves;
[0080] 2) Repeat the leaching of the mulberry leaf filter residue once according to step 1), and mix the 1-DNJ preliminary extract obtained twice;
[0081] 3) The mixed 1-DNJ preliminary extract was mixed and concentrated by rotary evaporation, then centrifuged at 5000rpm for about 15min, the supernatant was collected, suction filtered, and the filtrate was collected;
[0082] 4) Dilute the filtrate with ultrapure water to 0....
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Abstract
The invention discloses a response surface method optimized method for extracting 1-deoxynojirimycin (1-DNJ) in mulberry leaves with an acidic ethanol solution. The method is characterized in that the acidic ethanol solution is taken as the extraction solvent for extracting the 1-DNJ in the mulberry leaves, and the extraction condition is optimized by the response surface method so that the optimal condition is obtained, namely, the solution-to-material ratio is 25, and in other words, 25mL of extraction solvent is used for each gram of crude mulberry leaf powder; the method comprises the steps of extracting for 2.7h under the condition of 80 DEG C, re-extracting once, purifying the filtrate, and then concentrating the filtrate to obtain the 1-DNJ extract; the method is capable of obtaining about 0.2% of mulberry leaf 1-DNJ extraction rate, which is remarkably higher than the traditional ethanol extraction rate 0.00139% and the diluted acid extraction efficiency 0.00147%; obviously, the diluted acid and the ethanol have synergistic effect in the mulberry leaf 1-DNH extraction process and unexpected effect is generated, and therefore, theoretical support and technical guidance are provided for development and utilization of the mulberry leaf 1-DNH in the aspects of medicine and healthcare products.
Description
technical field [0001] The invention relates to a method for extracting 1-deoxynojirimycin, in particular to a method for extracting 1-deoxynojirimycin from mulberry leaves with dilute acid ethanol optimized by response surface methodology, and belongs to the technical field of plant extraction. Background technique [0002] Mulberry leaf 1-deoxynojirimycin (1-DNJ) is a natural piperidine small molecule water-soluble alkaloid found in mulberry tree (Morus alba L.), with a molecular weight of 163.7. As a potent inhibitor of glucose metabolizing enzymes (such as α-glucosidase, hexokinase, glucuronidase and glycogen phosphatase, etc.), DNJ can significantly delay the degradation process of polysaccharides and reduce the peak blood sugar after meals. Stabilize fasting blood sugar. In addition, DNJ also has the effect of increasing insulin sensitivity and improving insulin resistance. [0003] Mulberry leaf 1-deoxynojirimycin (1-DNJ) belongs to piperidine small molecule water-s...
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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/46
CPCC07D211/46
Inventor 苏楠吴新荣
Owner GUANGZHOU GENERAL HOSPITAL OF GUANGZHOU MILITARY COMMAND
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