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Method for crudely extracting pleocidin

A spinosad, crude extraction technology, applied in the direction of chemical instruments and methods, biocides, chemicals for biological control, etc., can solve the problems of adsorption rate requirements, leakage, product purity not clearly stated, etc., to improve Recovery rate, organic solvent saving, effect of small elution volume

Inactive Publication Date: 2012-09-26
SHANGHAI INST OF PHARMA IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this resin leaks when it adsorbs spinosad at pH 5-11, it cannot achieve complete adsorption effect, and it also has higher requirements on the adsorption rate
In the study of desorption with this resin, the investigation of the desorption conditions (pH) only selected the static experiment, and the pH was not changed during the elution process of the dynamic experiment, and the obtained eluate also contained more obvious pigments. The purity of the product after stripping is not clearly stated

Method used

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  • Method for crudely extracting pleocidin
  • Method for crudely extracting pleocidin
  • Method for crudely extracting pleocidin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Embodiment 1: Static experiment compares adsorption resin:

[0034] Take 20ml each of the treated YPR-II and XAD-4 macroporous adsorption resins, put them into 750ml Erlenmeyer flasks respectively, then add 200ml of pretreated fermentation broth, place them on a shaking table at 28°C and 150r / min to vibrate and adsorb, Samples were taken at 3, 6, and 9 hours for HPLC titer determination. A total of 4 samples were added, and the volume of the fermentation broth added each time was 200ml. in,

[0035] Ratio of unadsorbed product = (sampling titer after adsorption / fermentation broth titer after pretreatment) × 100%

[0036] Table 2

[0037]

[0038] Table 2 shows that compared with XAD-4 resin, YPR-II resin has a faster adsorption rate and can achieve complete adsorption in a shorter time.

Embodiment 2

[0039] Embodiment 2: Adopt YPR-II resin to adsorb the fermentation broth after spinosad pretreatment, investigate the influence of pH on adsorption

[0040] 1) Adjustment of fermentation broth and resin column pH:

[0041] After pretreatment of the fermented liquid obtained according to the existing literature, each get 200ml, adjust the pH to 4.0, 5.0, 6.0, 7.0, 8.0, 9.0, 10.0, 11.0 respectively; get every 20ml of processed resin to pack into a resin column, and then Rinse the YPR-II resin column with acetone that has adjusted the corresponding pH, so that the pH of the resin reaches the pH of the pre-column fermentation broth, that is, resins with pHs of 4.0, 5.0, 6.0, 7.0, 8.0, 9.0, 10.0, and 11.0 column.

[0042] 2) Upper column:

[0043] Adsorb with corresponding pH resin columns on the pH-adjusted fermentation broth, collect in units of 50 ml, and detect the leakage rate by HPLC. in:

[0044] Leakage rate (%) = potency of each collection unit / potency of fermentation ...

Embodiment 3

[0050] Example 3: Comparison of eluents

[0051] Take 20ml of the adsorbed YPR-II resin and fix it in a column, then use 0%, 20%, 40%, 60%, 80%, 100% acetone and methanol to elute, and use 200ml of each concentration solution volume, and the eluate was collected as a unit for HPLC titer determination. The results are shown in Table 4 below:

[0052] Table 4

[0053]

[0054] As can be seen from the above table 4, the elution ability of acetone is stronger than that of methanol and acetone, and the highest peak can be reached when the concentration is 80%.

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Abstract

The invention discloses a method for crudely extracting pleocidin, which comprises the step of absorbing macroporous absorbent resin column YPR-II on the pretreated pleocidin fermentation liquor. The pleocidin eluent obtained by the method has high purity, less coloring matter content and high yield. The method has simple process and convenient operation.

Description

technical field [0001] The invention belongs to the technical field of biological pesticide production, and in particular relates to a method for crudely extracting spinosad. Background technique [0002] Spinosad is a novel macrolide ultra-high-efficiency biological source extracted from the fermentation broth of Saccharopolyspora spinosa isolated from the soil of the Virgin Islands in 1982 by researchers from the American Lilly Company. pesticides. Produced by the Dow Agricultural Sciences Company of the United States, the trade names registered in my country in 1999 are Tracer (48% suspension) and Caixi (Success 2.5% suspension), which are respectively used in the control of diamondback moth and cotton bollworm. Its active ingredients are Spinosyn A and D, wherein the proportions of A and D are 85% and 15% respectively. Spinosad is mainly used in the control of cotton bollworm, tobacco budworm, diamondback moth, fruit fly, beet armyworm, thrips, etc. It is suitable for ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/08C07H1/06A01P7/00
Inventor 李继安韩丽敏
Owner SHANGHAI INST OF PHARMA IND CO LTD
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