A simple and efficient method for treating crude abscisic acid mother liquor

Abstract

The invention discloses a simple and efficient method for treating abscisic acid crude product mother liquor, characterized in that: the treatment method comprises the following steps: pH adjustment of abscisic acid crude product mother liquor: abscisic acid crude product mother liquor is regulated pH with liquid alkali; stirring, filtering: stirring and mixing the mother liquor after adjusting pH and filtering through a filter bag; sampling and measuring titer: sampling the crude product mother liquor after filtration, detecting, measuring its titer, and the titer is generally 2000-3000ug / ml (titer is represented by u, unit ug / ml); calculating the required concentration or dilution multiple: calculating the mother liquor multiple that needs to be concentrated or diluted according to the required preparation concentration, calculation formula: the present invention is simple to operate, easy to implement, high processing efficiency, and economic and environmentally friendly, suitable for industrial production. Concentration multiples can be selected according to the required abscisic acid preparation concentration, and different preparation products are prepared. In this way, there will be no mother liquor residue, truly harmless treatment, and high processing efficiency, economic and environmentally friendly.

Description

Technical Field

[0001] The invention belongs to the field of plant growth regulators, and in particular relates to a simple and efficient method for treating abscisic acid crude mother liquor. The method is suitable for treating abscisic acid mother liquor. Background Art

[0002] Abscisic acid is a widely used plant growth regulator, which can not only improve the drought resistance and salt tolerance of plants, but also is an effective inhibitor of seed germination, which is of great value to desert greening and seed storage, ensuring that the storage quality of seeds and fruits is extremely high. In addition, abscisic acid is a key factor in balancing the metabolism of plant endogenous hormones and related bioactive substances, has the ability to promote balanced absorption of water, fertilizer and coordination of metabolism in the body of plants, can effectively regulate the root crown and nutritional growth of plants, and plays an important role in improving the quality and yield of crops. At present, the industry generally adopts microbial fermentation to produce abscisic acid, and the abscisic acid obtained is (+) ABA, which has the advantages of activity and high purity, but the problem is that there is also abundant organic matter in the abscisic acid feed liquid produced by the fermentation method, and these organic matters cannot be separated or separated during extraction. And the mother liquor produced cannot be processed, causing great waste.

[0003] At present, the industrial method for extracting abscisic acid is to filter the fermentation liquid through a plate and frame, and then perform membrane concentration. After concentrating to a certain multiple, a concentrated solution of abscisic acid is obtained, and the concentrated solution is adjusted to adjust the pH to precipitate coarse powder, and the subsequent coarse powder mother liquor is further extracted, or the concentrated solution is directly used for extraction. After the extraction is completed, it is concentrated under reduced pressure and chromatographically treated, and finally crystallized using petroleum ether. The entire extraction process is complicated, and a large amount of organic solvents petroleum ether and ethyl acetate are consumed, the mother liquor processing volume is large, and the efficiency is low. At the same time, most of the commercial abscisic acid products on the market are various types of abscisic acid preparations prepared using abscisic acid. These preparations are generally prepared using abscisic acid, various additives, solvents, and various trace organic minerals according to demand. In our extraction process, the coarse powder precipitated after the concentrated solution after membrane concentration is adjusted to pH can be directly processed into abscisic acid fine powder with a content of more than 90%. The effective ingredient in the coarse powder mother liquor is 2000-3000ug / ml, and it contains trace amounts of organic matter. We can use these mother liquors to prepare abscisic acid preparations of different concentrations after processing. This treatment method is simple to operate, easy to implement, can save a lot of costs, is highly efficient, and is environmentally friendly. Summary of the invention

[0004] In view of the deficiencies in the prior art, the present invention provides a simple and efficient method for treating abscisic acid crude mother liquor, which solves the above-mentioned problems.

[0005] To achieve the above object, the present invention is implemented by the following technical scheme: a simple and efficient method for treating crude abscisic acid mother liquor, the method comprising the following steps:

[0006] (1): pH adjustment of the crude abscisic acid mother liquor: The pH of the crude abscisic acid mother liquor is adjusted with liquid alkali;

[0007] (2): Stirring and filtering: Stir the mother liquor after adjusting the pH and then filter it through a filter bag;

[0008] (3): Sampling and titer measurement: Sampling the crude mother liquor after filtration, testing and measuring its titer, the titer is generally 2000-3000ug / ml (the titer is expressed in u, unit ug / ml);

[0009] (4): Calculate the required concentration or dilution multiple: Calculate the required concentration or dilution multiple of the stock solution based on the required preparation concentration. The calculation formula is: If n>1, it means that the potency of the mother solution is lower than the concentration of the prepared product, and the mother solution is concentrated. The concentration multiple is calculated as follows: w% represents the concentration of the preparation to be prepared, u represents the potency of the mother solution. If n<1, the potency of the mother solution is higher than the concentration of the preparation product to be prepared, and the mother solution needs to be diluted. The dilution multiple is calculated as follows: If n = 1, no concentration or dilution is required;

[0010] (5): Concentrate or dilute under reduced pressure: Concentrate or dilute under reduced pressure according to the concentration or dilution multiple calculated in the above step, until the concentration or dilution reaches the required multiple;

[0011] (6): Storage and preparation of preparations.

[0012] Furthermore, the pH value in step (1) is adjusted to 5.0-7.0 using liquid alkali.

[0013] Furthermore, the stirring and mixing time in step (2) is 30 min-60 min.

[0014] Furthermore, the detection equipment in step (3) is a liquid chromatograph, and the detection method uses a standard curve method.

[0015] Furthermore, the reduced pressure concentration temperature in step (5) is controlled at about 60 to 80° C., the vacuum degree is controlled at -0.08 to -0.10 MPa, the instrument used is a rotary evaporator or a reduced pressure concentration evaporator, the solvent used for dilution is deionized water, and the concentration or dilution multiple is calculated based on the concentration of the desired preparation.

[0016] Beneficial Effects

[0017] The present invention provides a simple and efficient method for treating abscisic acid crude mother liquor. Compared with the prior art, it has the following beneficial effects:

[0018] The invention is simple to operate, easy to implement, has high processing efficiency, is economical and environmentally friendly, and is suitable for industrial production. The concentration multiple can be selected according to the required abscisic acid preparation concentration to prepare different preparation products. In this way, there will be no mother liquor residue, and harmless treatment is truly achieved, and the processing efficiency is high, which is economical and environmentally friendly. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 It is a process flow chart of the present invention. DETAILED DESCRIPTION

[0020] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0021] Please refer to the accompanying drawings, the present invention provides Example 1:

[0022] 1) pH adjustment of crude abscisic acid mother liquor;

[0023] Take 100 ml of crude abscisic acid mother liquor with a titer of 2400 ug / ml, use liquid alkali to adjust the pH to 6.57, and proceed to the next step.

[0024] 2) Stirring and filtering

[0025] The pH of the abscisic acid crude mother liquor was adjusted, stirred for 30 minutes, and then filtered using filter paper and a Bush funnel to obtain 96.52 ml of a pale yellow crude mother liquor.

[0026] 3) Sampling and titer measurement

[0027] The filtered abscisic acid mother liquor was obtained, and a sample was taken for potency measurement, and a liquid chromatograph was used for detection. The detection method used a standard curve method, and the potency of the obtained crude mother liquor was 2467ug / ml.

[0028] 4) Calculate the required concentration or dilution multiple

[0029] To prepare a 0.03% abscisic acid preparation, use the formula: We get n = 0.12 < 1, that is, the mother liquor content is relatively high compared to the abscisic acid content of the preparation we need to prepare. The dilution factor is 8.2 times.

[0030] 5) Concentrate or dilute under reduced pressure

[0031] It is calculated from the fourth step that when preparing a 0.03% abscisic acid preparation, since the concentration of the prepared preparation is too low, we do not need to concentrate it, but need to add 8.2 times the volume of the original mother liquor for dilution, that is, add 791.46 ml of filler for dilution. The final 881.90 ml of mother liquor was tested to have a potency of 271.31 ug / ml, which meets the requirements for preparing a 0.03% abscisic acid preparation.

[0032] 6) Storage and preparation of preparations:

[0033] The abscisic acid mother solution that has been calculated to be needed to prepare the 0.03% abscisic acid preparation is labeled with the concentration of the prepared preparation and the multiple of dilution required for subsequent preparation.

[0034] Embodiment 2:

[0035] 1) pH adjustment of crude abscisic acid mother liquor

[0036] Take 100 ml of crude abscisic acid mother liquor with a titer of 2745 ug / ml, use liquid alkali to adjust the pH to 6.73, and proceed to the next step.

[0037] 2) Stirring and filtering

[0038] The pH of the abscisic acid crude mother liquor was adjusted, stirred for 40 minutes, and then filtered using filter paper and a Bush funnel to obtain 95.31 ml of a pale yellow crude mother liquor.

[0039] 3) Sampling and titer measurement

[0040] The filtered abscisic acid mother liquor was obtained, and a sample was taken for potency measurement, and a liquid chromatograph was used for detection. The detection method used a standard curve method, and the potency of the crude mother liquor obtained was 2873ug / ml.

[0041] 4) Calculate the required concentration or dilution multiple

[0042] To prepare a 0.1% abscisic acid preparation, use the formula: We get n = 0.34 < 1, that is, the mother liquor content is relatively high compared to the abscisic acid content of the preparation we need to prepare. The dilution factor required is 2.87 times.

[0043] 5) Concentrate or dilute under reduced pressure:

[0044] It is calculated from the fourth step that when preparing a 0.1% abscisic acid preparation, due to the low concentration of the prepared preparation, we do not need to concentrate it, but need to add 2.87 times the volume of the original mother liquor for dilution, that is, add 273.51 ml of filler for dilution. The final 366.52 ml of mother liquor was tested to have a potency of 271.31 ug / ml, which meets the requirements for preparing a 0.03% abscisic acid preparation.

[0045] 6) Barreling, storage and preparation of preparations:

[0046] The abscisic acid mother solution that has been calculated to be needed to prepare the 0.03% abscisic acid preparation is labeled with the concentration of the prepared preparation and the multiple of dilution required for subsequent preparation.

[0047] Embodiment 3:

[0048] 1) pH adjustment of crude abscisic acid mother liquor

[0049] Take 2000ml of crude abscisic acid mother liquor with a titer of 2890ug / ml, use liquid alkali to adjust the pH to 6.86, and proceed to the next step.

[0050] 2) Stirring and filtering

[0051] After adjusting the pH, the crude mother liquor of abscisic acid was stirred for 50 min and then filtered with filter paper and Bush funnel to obtain a pale yellow crude mother liquor.

[0052] 3) Sampling and titer measurement

[0053] The filtered abscisic acid mother liquor was obtained, and a sample was taken to measure the potency, and a liquid chromatograph was used for detection, and the detection method used the standard curve method for detection, and the potency of the obtained crude mother liquor was 2932ug / ml. The volume of the obtained crude mother liquor was 1970ml.

[0054] 4) Calculate the required concentration or dilution multiple

[0055] To prepare a 2.5% abscisic acid preparation, use the formula: It is obtained that n=8.5>1, that is, the content of the mother liquor is relatively low compared with the abscisic acid content of the preparation we need to prepare, and the mother liquor needs to be concentrated. The calculation formula for the concentration multiple is: It is calculated that n=8.5, which means that the crude mother liquor needs to be concentrated 8.5 times, and the volume of the crude mother liquor after concentration is approximately 394.27 ml.

[0056] 5) Concentrate or dilute under reduced pressure

[0057] It is calculated from the fourth step that when preparing a 2.5% abscisic acid preparation, we need to concentrate the crude mother liquor by 8.5 times, that is, the volume of the mother liquor is concentrated from 1970ml to 207.4ml. Use a rotary evaporator for concentration, the concentration temperature is 65°C, the vacuum degree is -0.09MPa, and the concentration time is 72min. The final remaining mother liquor volume is 397.62ml. Samples were taken to measure the potency, and the potency was 27846ug / ml, which meets the concentration requirements for preparing a 2.5% abscisic acid preparation.

[0058] 6) Barreling, storage and preparation of preparations:

[0059] The abscisic acid mother solution that has been calculated to be needed to prepare the 2.5% abscisic acid preparation is labeled with the concentration of the prepared preparation and the multiple of dilution required for subsequent preparation.

[0060] Example 4: Industrialization Example

[0061] 1) pH adjustment of crude abscisic acid mother liquor

[0062] The 3000L crude mother liquor of abscisic acid just filtered had a potency of 2578ug / ml. Liquid alkali was used to adjust the pH to 6.92 for the next step.

[0063] 2) Stirring and filtering

[0064] The pH of the abscisic acid crude mother liquor was adjusted, stirred for 55 minutes, and then passed through a bag filter with a filter bag to obtain a light yellow crude mother liquor.

[0065] 3) Sampling and titer measurement

[0066] The filtered abscisic acid mother liquor was obtained, and a sample was taken to measure the potency, and a liquid chromatograph was used for detection, and the detection method used the standard curve method for detection, and the potency of the obtained crude mother liquor was 2634ug / ml. The volume of the obtained crude mother liquor was 2924L.

[0067] 4) Calculate the required concentration or dilution multiple

[0068] To prepare a 0.03% abscisic acid preparation, use the formula: We get n = 0.11 < 1, that is, the mother liquor content is relatively high compared to the abscisic acid content of the preparation we need to prepare. The dilution factor is 8.8 times.

[0069] 5) Concentrate or dilute under reduced pressure

[0070] From the calculation in step 4, we know that when preparing 0.03% abscisic acid preparation, because the concentration of the prepared preparation is too low, we do not need to concentrate it, but need to add 8.8 times of filler for dilution. That is, we need to use 25731L of deionized water for dilution. After dilution, we take samples to measure the potency, and the potency is 277ug / ml, which meets the concentration requirements of the prepared abscisic acid preparation.

[0071] 6) Storage and preparation of preparations:

[0072] The abscisic acid mother solution that has been calculated to be needed to prepare the 0.03% abscisic acid preparation is labeled with the concentration of the prepared preparation and the multiple of dilution required for subsequent preparation.

[0073] Example 5: Industrialization Example

[0074] 1) pH adjustment of crude abscisic acid mother liquor

[0075] The 3000L crude mother liquor of abscisic acid just filtered had a potency of 2789ug / ml. Liquid alkali was used to adjust the pH to 6.96 for the next step.

[0076] 2) Stirring and filtering

[0077] The pH of the abscisic acid crude mother liquor was adjusted, stirred for 60 minutes, and then passed through a bag filter with a filter bag to obtain a light yellow crude mother liquor.

[0078] 3) Sampling and titer measurement

[0079] The filtered abscisic acid mother liquor was obtained, and a sample was taken to measure the potency, and a liquid chromatograph was used for detection, and the detection method used the standard curve method for detection, and the potency of the obtained crude mother liquor was 2852ug / ml. The volume of the obtained crude mother liquor was 2932L.

[0080] 4) Calculate the required concentration or dilution multiple

[0081] To prepare a 2.5% abscisic acid preparation, use the formula: We get n=8.8>1, that is, the mother liquor content is relatively low compared to the abscisic acid content of the preparation we need to prepare, and the mother liquor needs to be concentrated. The calculation formula for the concentration multiple is: It is calculated that n=8.5, which means that the crude mother liquor needs to be concentrated 8.8 times, and the remaining mother liquor volume is approximately 333.18L.

[0082] 5) Concentrate or dilute under reduced pressure

[0083] According to the calculation in step 4, when preparing a 2.5% abscisic acid preparation product, we need to concentrate the crude mother liquor by 8.5 times, that is, the volume of the mother liquor is concentrated from 1970ml to 207.4ml. Use a vacuum concentration evaporator for concentration, the concentration temperature is 70°C, the vacuum degree is -0.09MPa, and the concentration time is 84min. The remaining mother liquor volume is 342.56L. Samples were taken to measure the potency, and the potency was 24782ug / ml, which meets the concentration requirements for preparing a 2.5% abscisic acid preparation.

[0084] 6) Storage and preparation of preparations:

[0085] The abscisic acid mother solution that has been calculated to be needed to prepare the 2.5% abscisic acid preparation is labeled with the concentration of the prepared preparation and the multiple of dilution required for subsequent preparation.

Claims

1. A simple method for treating crude abscisic acid mother liquor, characterized in that: The processing method comprises the following steps: (1): pH adjustment of the crude abscisic acid mother liquor: the pH of the crude abscisic acid mother liquor is adjusted with liquid alkali; the adjusted pH is 5.0-7.0; (2): Stirring and filtering: Stirring and mixing the mother liquor after adjusting the pH and then filtering it through a filter bag; the stirring and mixing time is 30min-60min; (3): Sampling and titer measurement: Sampling the crude mother liquor after filtration, testing and measuring its titer, the titer is generally 2000-3000ug / ml (the titer is expressed in u, unit ug / ml); (4): Calculate the required concentration or dilution multiple: Calculate the required concentration or dilution multiple of the stock solution based on the required preparation concentration. The calculation formula is: n=w% / u*10 6 If n>1, it means that the potency of the mother solution is lower than the concentration of the prepared product, so the mother solution is concentrated. The concentration multiple is calculated as follows: n=w% / u*10 6 , w% represents the concentration of the preparation to be prepared, u represents the potency of the mother solution. If n<1, the potency of the mother solution is higher than the concentration of the preparation product to be prepared, and the mother solution needs to be diluted. The dilution multiple calculation formula is: n=u / w%*10 -6 ,If n=1, no concentration or dilution is needed; (5): Concentrate or dilute under reduced pressure: Concentrate or dilute under reduced pressure according to the concentration or dilution multiple calculated in the above step, until the concentration or dilution reaches the required multiple; (6): Storage and preparation of preparations.

2. The method for treating abscisic acid crude product mother liquor according to claim 1, characterized in that: The detection equipment described in step (3) is a liquid chromatograph, and the detection method used is a standard curve method.

3. The method for treating the crude abscisic acid mother liquor according to claim 1, characterized in that: The reduced pressure concentration temperature in step (5) is controlled at 60 to 80° C., the vacuum degree is controlled at -0.08 to -0.10 MPa, the instrument used is a rotary evaporator or a reduced pressure concentration evaporator, the solvent used for dilution is deionized water, and the concentration or dilution multiple is calculated based on the concentration of the desired preparation.

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