Low-pesticide residue ginseng stem leaf extract and preparation method thereof

A technology of ginseng stems and leaves and extracts, which is applied in the direction of pharmaceutical formulas, plant raw materials, medical preparations containing active ingredients, etc., can solve problems such as low yield, waste of reagents, and environmental pollution, and achieve easy operation and high production technology. easy effect

Active Publication Date: 2018-05-18
杨凌萃健生物工程技术有限公司
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AI-Extracted Technical Summary

Problems solved by technology

[0016] The existing patent application number CN104490966A discloses a method for removing residual pesticides in ginseng stem and leaf extracts; the method extracts ginseng stem and leaf total saponins aqueous solution by mixing organic solvents, and then dilutes the mother liquor through macroporous resin, 65-80 % elution, collect the eluate, and dry to obtain the finished product; but this process does not mention obstinate pesticides, such as propamocarb, oxaxyl, etc., and the mixed solvent used is difficult to recycle and reuse, resulting in waste an...
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Abstract

The invention discloses a low-pesticide residue ginseng stem leaf extract and a preparation method thereof. The method comprises the following steps that 1, ethanol extraction: ginseng stem leaves aretaken to be pulverized into coarse powder, ethanol is added and heated, refluxing extraction is conducted twice, filtering is conducted, filtrates are combined, decompression concentration is conducted, and water is added for concentration until smell of the ethanol is completely removed to obtain concentrated liquid; 2 impurity removal: impurity removal is conducted on the concentrated liquid obtained in step 1, centrifugal filtration is conducted, and supernatant liquid is obtained; 3, purification: decompression concentration is conducted on the supernatant liquid obtained in step 2, concentration is conducted to obtain extract, methanol solution is added, filtering is conducted by using filter paper, the filtrate is subjected to gel column chromatography to collect lower column liquids, thin-layer chromatography is adopted for detection, the lower column liquids with Rg1, Re and Rd spots are combined, and decompression concentration, drying and pulverizing are conducted to obtainthe low-pesticide residue ginseng stem leaf extract. According to the extract, ginsenoside content in a ginseng stem leaf extract prepared through the method is high, pesticide residue is low, whereinthe ginsenoside content (Rg1, Re and Rd) is larger than or equal to 65%, and the pesticide residue indexes conform to an EC396 standard.

Application Domain

Plant ingredients

Technology Topic

Thin-layer chromatographyChemistry +11

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  • Low-pesticide residue ginseng stem leaf extract and preparation method thereof

Examples

  • Experimental program(3)
  • Comparison scheme(2)

Example Embodiment

[0051] Example 1
[0052] 500g ginseng stems and leaves were crushed into 20 mesh coarse powder, and 90% ethanol was added for reflux extraction twice. The amount of ethanol added each time was 10 and 8 times the mass of ginseng stems and leaves. The extraction time was heated and refluxed at 150°C. 2 and 1.5h, filtered with 200 mesh filter cloth, combined the filtrate, -0.09MPa reduced pressure and concentrated, supplemented with water and concentrated until no alcohol, put it in the refrigerator at 4℃ for 12h, centrifuged and filtered, take the supernatant -0.09MPa reduced pressure and concentrate to The extract is dissolved in 100ml methanol, filtered with filter paper, and the filtrate is subjected to SephadexLH-20 (manufacturer: Shanghai Baoman Biotechnology Co., Ltd.) gel column chromatography at a flow rate of 5s per drop, and each 50ml is used as a fraction to collect the lower column liquid. Detect by thin layer chromatography, draw 2μL each of the lower column solution and the reference substance (Beijing Zhongke Quality Inspection Biotechnology Co., Ltd.), and place them on the same silica gel G thin layer plate, and use chloroform-ethyl acetate- Methanol-water (15:40:22:10) The lower layer solution placed below 10℃ is the developing agent. After unfolding, air dry, spray with 10% sulfuric acid ethanol solution, heat at 105℃ until the spots appear clear, and place them in sunlight. And inspect under ultraviolet light (365nm), combine the bottom column liquid with Rg1, Re, Rd spots, concentrate under reduced pressure, and dry under vacuum to obtain low pesticide residue ginseng stem and leaf extract.

Example Embodiment

[0053] Example 2
[0054] Take 600g of ginseng stems and leaves and crush them into 24 mesh coarse powder, add 80% ethanol and reflux for extraction twice. The amount of ethanol added each time is 10 times and 8 times the mass of ginseng stems and leaves. The extraction time is heated and refluxed at 150℃. 2 and 1.5h, filtered with 200 mesh filter cloth, combined the filtrate, -0.08MPa reduced pressure and concentrated, supplemented with water and concentrated to no alcohol, put it in the refrigerator at 4℃ for 8h, centrifuged and filtered, and took the supernatant -0.08MPa reduced pressure and concentrated to Extract the extract, add 100ml methanol to dissolve it, filter it with filter paper, pass the filtrate to SephadexLH-20 gel column chromatography at a flow rate of 5s per drop, with each 60ml as a fraction to collect the lower column liquid, use thin-layer chromatography to detect, draw each fraction 2μL each of column solution and reference substance, respectively spot on the same silica gel G thin-layer plate, use chloroform-ethyl acetate-methanol-water (15:40:22:10) lower layer solution placed below 10℃ as developing agent After unfolding, air dry, spray with 10% sulfuric acid ethanol solution, heat at 105℃ until the spots are clearly colored, and inspect under sunlight and ultraviolet light (365nm) respectively, and combine the lower column liquid with Rg1, Re, and Rd spots , Concentrated under reduced pressure and dried in vacuum to obtain low pesticide residue ginseng stem and leaf extract.

Example Embodiment

[0055] Example 3
[0056] Take 1000g ginseng stems and leaves and crush them into 24 mesh coarse powder, add 70% ethanol and reflux for extraction twice. The amount of ethanol added each time is 10 times and 8 times the mass of ginseng stems and leaves. The extraction time is heated and refluxed at 160℃. 2 and 1.5h, filter with 200 mesh filter cloth, combine the filtrate, -0.08MPa reduced pressure and concentrate, make up water and concentrate until there is no alcohol, put it in the refrigerator at 4℃ for 10h, centrifuge and filter, take the supernatant and concentrate -0.08MPa under reduced pressure to Extract the extract, add 200ml methanol to dissolve, filter with filter paper, pass the filtrate to Sephadex G-10 (manufacturer: Shanghai Baoman Biotechnology Co., Ltd.) gel column chromatography, flow rate 6 seconds per drop, with each 100ml as a fraction to collect the lower column liquid , Using thin-layer chromatography to detect, draw 2μL each of the lower column liquid and the reference substance, and place them on the same silica gel G thin layer plate, and use chloroform-ethyl acetate-methanol-water (15:40:22: 10) The lower layer solution placed below 10℃ is a developing agent. After unfolding, air dry, spray with 10% sulfuric acid ethanol solution, heat at 105℃ until the spots appear clear, and inspect under sunlight and ultraviolet light (365nm) respectively. The lower column liquid with Rg1, Re, and Rd spots is combined, concentrated under reduced pressure, and dried in vacuum to obtain a low-residue ginseng stem and leaf extract.

PUM

PropertyMeasurementUnit
Mesh20.0 ~ 30.0mesh

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