阅读说明：本技术 一种基于结晶技术去除蜂王浆浆渣中异物的方法 (Method for removing foreign matters in royal jelly slurry residue based on crystallization technology ) 是由 周萍 于 2021-08-11 设计创作，主要内容包括：本发明提供了一种基于结晶技术去除蜂王浆浆渣中异物的方法,包括往蜂王浆浆渣加入95％食用酒精通过刮滤、磁捧吸附、蒸发浓缩、过400目筛网等步骤得精制浆渣；该方法能大大提高浆渣的纯度,最大限度减少了浆渣中的异物,不增加外来成分,从而提高产品品质,同时免去了人工挑选浆渣带来的人工成本和浆渣挑选品质的不稳定性,值得在实际生产中推行。(The invention provides a method for removing foreign matters in royal jelly pulp residue based on crystallization technology, which comprises the steps of adding 95 percent edible alcohol into the royal jelly pulp residue, scraping and filtering, magnetically holding and adsorbing, evaporating and concentrating, sieving by a 400-mesh sieve and the like to obtain refined pulp residue; the method can greatly improve the purity of the pulp slag, reduces foreign matters in the pulp slag to the maximum extent, does not increase foreign components, thereby improving the product quality, simultaneously avoids the labor cost caused by manually selecting the pulp slag and the instability of the pulp slag selection quality, and is worthy of being implemented in the actual production.)

1. A method for removing foreign matters in royal jelly slurry residue based on crystallization technology is characterized by comprising the following steps:

1) adding 95% edible alcohol into Lac Regis Apis slurry residue, stirring for dissolving, adding purified water, stirring for dissolving, sieving with 120 mesh nylon sieve by scraping, filtering with magnetic rod to adsorb foreign matter, sieving with 200 mesh nylon sieve by scraping, and filtering with magnetic rod to adsorb foreign matter to obtain filtrate without foreign matter;

2) adding purified water into the obtained filtrate without foreign matters, mixing, rotary evaporating for concentration until the distilled liquid has no ethanol, pouring out the material, washing the inner wall with water, mixing with the material, placing in a 0-5 deg.C refrigerator, storing overnight, taking out the material, passing through a 400 mesh screen with purified slurry residue on the upper part;

or the like, or, alternatively,

2') adding purified water into the obtained filtrate, stirring and mixing, placing in a refrigeration house at 0-5 ℃, storing overnight, passing through a 400-mesh nylon screen with available pulp residue on the upper part of the screen, collecting the available pulp residue, adding water and leaching until no ethanol smell exists, thus obtaining refined pulp residue;

the mass ratio of the royal jelly residues, the 95% edible alcohol and the purified water in the step 1) is 1:1: 0.667-1.

2. The method for removing foreign matter in royal jelly slurry residue based on crystallization technology according to claim 1, characterized in that the royal jelly slurry residue is residue of filtered royal jelly raw material, is rich in royal jelly acid 10-HDA peculiar to royal jelly, and has a moisture content of 40% -60%.

3. The method for removing foreign matters in royal jelly slurry residue based on crystallization technology according to claim 1, wherein the number of the magnetic rods in step 1) is 6, and the magnetic forces of the magnetic rods are more than or equal to 7000 gauss.

4. The method for removing foreign matters in royal jelly slurry residue based on crystallization technology according to claim 1, wherein the rotary evaporation concentration is performed under the conditions of 45-50 ℃ and 0.09MPa in the step 2).

Technical Field

The invention belongs to the field of royal jelly health-care products, and particularly relates to a method for removing foreign matters in royal jelly residues.

Background

The royal jelly residue is residue of royal jelly filtered by 100 mesh screen, as shown in figure 1, and contains about 20-40% of royal jelly acid-10-HDA, which is natural effective substance existing in royal jelly only in nature and is quality index and marker component index of royal jelly.

As the royal jelly slurry residue is rich in 10-HDA, the royal jelly slurry residue must be returned to the raw materials in the processing process, so as to meet the requirements of customers or national standards on the 10-HDA quality index. The royal jelly residue contains a large amount of impurities including wax scraps and other foreign matters (metal foreign matters and small black spots) besides effective components such as organic acids such as 10-HDA and the like, proteins and the like, and the royal jelly residue needs to be purified, otherwise the quality of products is influenced. The impurity content of filtered pulp residue of royal jelly produced in different producing areas and seasons has great difference.

Practice proves that foreign matters in the royal jelly pulp residue cannot be completely removed by the absorption of the magnetic rod, and particularly, the non-metal foreign matters are difficult to remove by the absorption of the magnetic rod. The conventional treatment means for impurities in the pulp residue in the prior art is to wash the pulp residue with water, sieve the pulp residue with a thicker 10-20-mesh sieve, wherein the sieve is residue, the main component is wax scraps, the lower part is a usable part and contains 10-HDA (royal jelly efficacy substance), meanwhile, smaller foreign matters also pass through the sieve, and the lower part of the royal jelly pulp residue is placed on a 120-mesh sieve to be squeezed by hands to obtain the washed pulp residue which needs to be further manually selected to be foreign matters visible to the naked eyes, so that purified pulp residue is obtained and then used for production. The production of the pulp slag can undoubtedly increase the labor cost, the pulp slag purification effect is unstable, the non-metallic foreign matters in the pulp slag, mainly small black spots, cannot be removed and are brought into the product, and the quality problem is caused.

Disclosure of Invention

Aiming at the defects in the prior art, the invention provides a method for removing foreign matters in royal jelly pulp residue based on a crystallization technology, which is simple and quick, and the pulp residue is pure and light yellow in crystal, and has no ethanol or foreign matters.

In order to realize the purpose of the invention, the invention adopts the following technical scheme:

a method for removing foreign matters in royal jelly slurry residue based on crystallization technology comprises the following steps:

1) adding 95% edible alcohol into Lac Regis Apis slurry residue, stirring for dissolving, adding purified water, stirring for dissolving, sieving with 120 mesh nylon sieve, sieving with 200 mesh nylon sieve, and sieving with magnetic rod to adsorb foreign matter to obtain filtrate;

2) adding purified water into the obtained filtrate, mixing, rotary evaporating for concentration until the distilled liquid has no ethanol, pouring out the material, washing the inner wall with water, mixing with the material, placing in 0-5 deg.C refrigerator, storing overnight, taking out the material, sieving with 400 mesh sieve, and collecting the purified slurry residue on the upper part of the sieve;

or the like, or, alternatively,

2') adding purified water into the obtained filtrate, stirring and mixing, placing in a refrigeration house at 0-5 ℃, storing overnight, passing through a 400-mesh nylon screen with available pulp residue on the upper part of the screen, collecting the available pulp residue, adding water and leaching until no ethanol smell exists, thus obtaining refined pulp residue;

the mass ratio of the royal jelly residues, the 95% edible alcohol and the purified water in the step 1) is 1:1: 0.667-1.

Further, in the step 1), the mass ratio of the royal jelly residues, the 95% edible alcohol and the purified water is 1:1-3: 1.

Furthermore, the royal jelly residue is residue obtained by filtering royal jelly raw material, is rich in royal jelly acid 10-HDA which is peculiar to royal jelly, and has the water content of 40-60%.

Furthermore, the number of the magnetic rods in the step 1) is 6, and the magnetic force of the magnetic rods is more than or equal to 7000 gausses.

Further, the step 2) is carried out rotary evaporation concentration under the conditions of 45-50 ℃ and 0.09 MPa.

The invention relates to selection of mesh number of a screen:

the foreign matters in the royal jelly dregs have different properties and sizes. 10-HDA is insoluble in water and can be dissolved in ethanol, 95% edible alcohol can quickly dissolve 10-HAD, and 10-HDA is dissolved into transparent solution for absolutely removing foreign matters, and then filtered by a screen with a certain mesh number. Considering that the requirements of customers for metal foreign matters in the product are less than 0.2mm, and the aperture size of the 100-mesh screen is 0.109mm, the requirements of the production process are completely met, and tests show that the operation of filtering by using the 100-mesh screen is feasible. The slurry residue solution can be filtered by adopting a 120-mesh → 200-mesh procedure, and the obtained product has less foreign matters.

Although the process for removing the metal foreign matters in the royal jelly production process is carried out for 3-5 times, the royal jelly needs to be adjusted by using the pulp residue to adjust the content of 10-HDA, and the pulp residue is a main source of small black spot foreign matters in the royal jelly product. The small black spots are one of indexes of foreign matters in the product, and each 100g of the small black spots is required to be less than 30, and the small black spots visible to naked eyes can be completely removed by filtering through a 200-mesh screen.

Meanwhile, in the existing pulp slag treatment process, a large amount of manpower is needed to select small black spots and other foreign matters in the pulp slag, the selection operation is very manual, the selection effect is different from person to person, and the method has the advantage that the manpower can not be replaced.

Determination of the sludge solvent:

the pulp residue contains 10-HDA as main component, wax bits, and small amount of protein and other impurities. The solubility of 10-HDA in ethanol of different concentrations is shown in Table 2

TABLE 1 10-HDA solubilization in ethanol of different concentrations

Concentration of ethanol	Processing method	10-HDA，％	Residue, g
				0％	10g of pulp residue	22.1	10
20％	10g of pulp residue → 20g of water → 80g of ethanol	0.47	4.5
				30％	10g of pulp → 30g of water → 70g of ethanol	1.59	3.3
40％	10g of pulp → 40g of water → 60g of ethanol	2.09	2.6
				50％	10g of pulp → 50g of water → 50g of ethanol	2.07	2.2

Therefore, more than 40% of ethanol can completely dissolve 10-HDA, and the optimal yield can be obtained by dissolving the pulp residue with 50% of ethanol. Considering that 40% is the critical ethanol concentration with high solubility of 10-HDA, and the concentration difference may cause the loss due to the too low solubility of 10-HAD in the production and preparation processes, the research adopts 50% ethanol to dissolve the pulp residue, so that the high solubility of 10-HAD can be ensured, and the yield is higher.

The method for removing the foreign matters in the royal jelly pulp residue can greatly improve the purity of the pulp residue, furthest reduce the foreign matters in the pulp residue, and does not increase external components, thereby improving the product quality, simultaneously avoiding the labor cost and the instability of the pulp residue selection quality caused by manually selecting the pulp residue, and being worthy of being promoted in the actual production.

Drawings

FIG. 1 is a diagram of untreated royal jelly sludge;

FIG. 2 is a graph of royal jelly dregs obtained by the treatment of example 1;

FIG. 3 is a picture of royal jelly dregs obtained by the treatment of example 3;

FIG. 4 is a diagram of royal jelly sludge obtained by the treatment of comparative example;

FIG. 5 is a diagram showing foreign matters in the sludge obtained in example 1, wherein black matters in the diagram are foreign matters;

FIG. 6 is a diagram showing foreign matters in the sludge obtained in the comparative example, wherein black matters in the diagram are foreign matters.

Detailed Description

The technical scheme of the invention is further described in detail by the following specific embodiments in combination with the attached drawings:

example 1

Weighing 10kg of royal jelly pulp, adding 10kg (95%) of edible alcohol, stirring for dissolving, adding 6.67kg of purified water, stirring for dissolving, sieving with a 120-mesh nylon sieve, performing scraping filtration by using 6 magnetic rods to adsorb foreign matters (the magnetic force of the magnetic rods is more than or equal to 7000 gauss), continuously sieving the obtained filtrate with a 200-mesh nylon sieve, performing scraping filtration by using 6 magnetic rods to adsorb foreign matters (the magnetic force of the magnetic rods is more than or equal to 7000 gauss) to obtain filtrate, adding 10kg of purified water into the filtrate, performing rotary evaporation concentration at 45 ℃ and 0.09MPa until the distilled liquid is free of ethanol, pouring out the material, washing the inner wall with water, adding the filtrate into the material, placing the material in a 0-5 ℃ refrigeration house, storing overnight, taking out the material, sieving with a 400-mesh sieve, collecting 8.88kg of pulp on the upper part of the sieve, and showing in figure 3.

Example 2

Weighing 10kg of royal jelly pulp, adding 10kg (95%) of edible alcohol, stirring for dissolving, adding 10kg of purified water, stirring for dissolving, sieving with a 120-mesh nylon sieve, performing scraping filtration by using 6 magnetic rods to adsorb foreign matters (the magnetic force of the magnetic rods is more than or equal to 7000 gauss), continuously sieving the obtained filtrate with a 200-mesh nylon sieve, performing scraping filtration by using 6 magnetic rods to adsorb foreign matters (the magnetic force of the magnetic rods is more than or equal to 7000 gauss) to obtain filtrate, adding 10kg of purified water into the filtrate, performing rotary evaporation concentration at 45 ℃ and 0.09MPa until the distilled liquid is free of ethanol, pouring out the material, washing the inner wall with water, putting into a 0-5 ℃ refrigeration house, storing overnight, taking out the material, sieving with a 400-mesh sieve, collecting 8.65kg of pulp on the upper part of the sieve.

Example 3

Weighing 10kg of royal jelly pulp, adding 10kg (95%) of edible alcohol, stirring for dissolving, adding 8.6kg of purified water, stirring for dissolving, sieving with a 120-mesh nylon sieve, performing scraping filtration by using 6 magnetic rods to adsorb foreign matters (the magnetic force of the magnetic rods is more than or equal to 7000 Gauss), continuously sieving the obtained filtrate with a 200-mesh nylon sieve, performing scraping filtration by using 6 magnetic rods to adsorb foreign matters (the magnetic force of the magnetic rods is more than or equal to 7000 Gauss), adding 20kg of purified water into the obtained filtrate, stirring and mixing, placing in a 0-5 ℃ refrigerator, standing overnight, taking out materials, sieving with a 400-mesh sieve to obtain usable pulp on the upper part of the sieve, wherein the pulp contains a small amount of ethanol, and repeatedly washing with water until no ethanol smell exists to obtain 8.67kg of refined pulp. See fig. 4.

Example 4

Weighing 10kg of royal jelly pulp, adding 10kg (95%) of edible alcohol, stirring for dissolving, adding 10kg of purified water, stirring for dissolving, sieving with a 120-mesh nylon sieve, performing scraping filtration by using 6 magnetic rods to adsorb foreign matters (the magnetic force of the magnetic rods is more than or equal to 7000 Gauss), further sieving with a 200-mesh nylon sieve, performing scraping filtration by using 6 magnetic rods to adsorb foreign matters (the magnetic force of the magnetic rods is more than or equal to 7000 Gauss), adding 40kg of purified water into the obtained filtrate, stirring and mixing, placing in a 0-5 ℃ refrigerator, storing overnight, taking out materials, sieving with a 400-mesh sieve to obtain usable pulp on the upper part of the sieve, wherein the pulp contains a small amount of ethanol, and repeatedly washing with water until no ethanol smell to obtain 8.53kg of refined pulp.

Comparison of example 1 and example 3 with respect to 10-HDA retention:

the 10-HDA is the characteristic component of the royal jelly and has positive correlation with the commodity price, and if the 10-HDA yield is too low in the treatment process, the method has defects and has no application value. Although 10-HDA has strong heat resistance, the research is a physical crystallization method, and the total amount of 10-HDA in the slurry residue cannot be lost, in view of the importance of 10-HDA, the research still examines two different post-treatment methods, namely the retention rate and the material balance of 10-HDA, the retention rate difference of the two post-treatment methods is larger, which is related to the concentration of ethanol, and dilute ethanol has higher solubility than water. The retention cases are shown in table 2.

TABLE 2 10-HDA Retention Rate profiles for different slurry and slag treatment methods

The data in this table is problematic in that the material is now 1 and 1 (20kg) in relation to alcohol, and then the residue plus filtrate is at least 10kg, and is now less than 9kg in addition

Comparative example (prior art)

Weighing 10kg of royal jelly pulp residue, adding 50kg of purified water, stirring and dissolving, screening by using a 10-20-mesh screen, wherein the screen is provided with residues, the main component is wax scraps, the lower part is an available part, the lower part of the royal jelly pulp residue is placed on a 120-mesh screen, and squeezing is carried out by hands to obtain washing pulp residue, the washing pulp residue needs to be further manually selected to obtain macroscopic foreign matters, so that the purified pulp residue is obtained, the method cannot remove the non-metallic foreign matters (mainly small black spots) in the pulp residue and bring the foreign matters into the product, so that the quality problem is caused, and the washing and purifying pulp residue is shown in figure 2.

The royal jelly residue treated by the prior art and the royal jelly residue treated by the technique are subjected to foreign matter detection, and the results are shown in figures 5 and 6. As can be seen from the figure, the foreign matters in the royal jelly residues treated by the prior art and the royal jelly residues treated by the technology have obvious difference seen by naked eyes, and the effect of removing the foreign matters by the technology is far better than that of the common prior art.