Preparation method and application of cherry pigment

Abstract

The invention belongs to the field of natural pigment preparation, and discloses a cherry pigment preparation method and application thereof, and the cherry pigment preparation method comprises the four steps of cherry extract preparation, macroporous resin extraction, concentration and drying. According to the method, fresh cherries are adopted as raw materials, a cherry extracting solution is obtained through cellulase enzymolysis, high-speed centrifugation and other processes, and finally cherry pigment powder is obtained through vacuum concentration and spray drying. The invention also discloses an application of the cherry pigment prepared by the method in preparation of a multi-color lipstick convenient to color, and a lipstick product which is bright in color and easy to color can be obtained through a specific formula and a preparation process. The method has the advantages of being environmentally friendly, high in cherry anthocyanin content, red and bright in obtained cherry pigment color, high in color value and the like, lipsticks of different color systems from bright red to red purple can be obtained only through one coloring agent and a small amount of pH adjusting agent in the lipstick preparation process, the requirements of the market for high-quality and natural-source lipstick products are met, and the market prospect is wide. Wide application prospects are realized.

Description

Technical Field

[0001] The invention belongs to the field of natural pigment preparation and discloses a preparation method of cherry pigment and application thereof. Background Art

[0002] As consumers become more aware of the potential health risks of artificial pigments, natural pigments are favored due to their green and safe sources and production processes, becoming an ideal alternative to synthetic pigments. Among the sources of natural pigments, plants dominate due to their abundant resources and safety, accounting for nearly 90% of the natural pigments allowed for use in my country. Plant natural pigments mainly include carotenoids, chlorophyll, betaine and anthocyanins. Anthocyanins, as a water-soluble flavonoid pigment widely found in fruits and vegetables, are not only safe and non-toxic, but also have nutritional value and health functions.

[0003] Cherries are stone fruits. Since the European sweet cherries were introduced to China in the 1970s, they have been widely planted in Shandong, Liaoning, Henan, Hubei, Sichuan, Shanxi and other places. At present, China's cherry industry has formed a considerable scale and production capacity. Cherries are rich in anthocyanins, which are the glycoside form of anthocyanidins. The content can reach up to 450mg / 100g fresh weight, and has significant antioxidant properties.

[0004] The softening of cherry fruits during ripening is a sign of their maturity, accompanied by the accumulation of flavor and nutrients. The increase in auxin (1-naphthylacetic acid) promotes the synthesis of anthocyanins, and the metabolism of carbohydrates converts starch into glucose, giving the fruit the ideal color and flavor. However, excessive softening can lead to a decrease in cherry flavor, weakened resistance, increased post-harvest losses, and shortened shelf life. Researchers are working on breeding and molecular studies to cultivate cherry varieties with longer shelf lives. At the same time, cherries with poor flavor after softening are still rich in anthocyanins. How to effectively utilize these resources and reduce waste and losses is an urgent problem to be solved. Summary of the invention

[0005] In order to solve the above problems, the present invention discloses a preparation method of cherry pigment and application thereof. The cherry pigment obtained by the method has high yield, high anthocyanin retention rate and bright color.

[0006] The present invention includes the following technical solutions:

[0007] A method for preparing cherry pigment, characterized in that it comprises the following steps:

[0008] (1) Preparation of cherry extract: fresh cherries are washed and pitted, and then crushed with a grinder at high speed to obtain cherry pulp. Cellulase is added to the cherry pulp and enzymatically hydrolyzed in a constant temperature water bath at 40-50° C. (preferably 45° C.). After the enzymatic hydrolysis is completed, the enzymatic hydrolyzate is centrifuged at 8000-12000 rpm (preferably 10000 rpm) for 10-30 min (preferably 20 min) and the bottom precipitate is removed to obtain a cherry extract;

[0009] (2) Macroporous resin extraction: The cherry extract obtained in (1) is subjected to a macroporous resin for pigment extraction, and then eluted with an edible ethanol aqueous solution to obtain a crude cherry pigment solution;

[0010] (3) Concentration: The crude cherry pigment solution obtained in (2) is concentrated under reduced pressure in a water bath at 60-70° C. (preferably 65° C.) and a vacuum degree of -0.08 to -0.1 MPa to obtain a concentrated cherry pigment paste;

[0011] (4) Drying: The obtained cherry pigment concentrated paste is spray-dried to obtain cherry pigment powder.

[0012] Furthermore, in the above-mentioned method for preparing cherry pigment, the cherry used in step (1) is one of Meizao, Black Pearl or Red Lantern.

[0013] Furthermore, in the above-mentioned method for preparing cherry pigment, the cellulase activity in step (1) is 50,000-150,000 IU (preferably 100,000 IU), the addition amount is 1-5 g / 10 kg, and the enzymatic hydrolysis time is 2-5 h.

[0014] Furthermore, in the above-mentioned method for preparing cherry pigment, the macroporous resin model in step (2) is XAD-7.

[0015] Furthermore, in the above-mentioned method for preparing cherry pigment, the concentration of the edible ethanol aqueous solution in step (2) is 30-60% (v / v).

[0016] Furthermore, in the above-mentioned method for preparing cherry pigment, the spray drying conditions in step (4) are an inlet air temperature of 150-200°C, an outlet air temperature of 80-100°C, and a flow rate of 5-15%; preferably, the spray drying conditions are an inlet air temperature of 180°C, an outlet air temperature of 90°C, and a flow rate of 10%.

[0017] The invention also discloses a cherry pigment which is prepared by the preparation method.

[0018] The invention also discloses the use of the cherry pigment in preparing a multi-color lipstick which is convenient for color adjustment.

[0019] Furthermore, in the above application, the method for preparing the lipstick comprises the following steps:

[0020] S1 Mix cherry pigment and grape seed oil and grind them in a grinder until the liquid is smooth and free of particles;

[0021] S2 Weigh water, lecithin, citric acid and sodium citrate, adjust the pH to 4.0-7.0, and stir in a water bath at 40-60° C. for 10-30 min; preferably, stir in a water bath at 50° C. for 20 min.

[0022] S3 heats and melts beeswax, mixes it with the liquid prepared by S1 and S2, heats it to 90-110° C. (preferably 100° C.), mixes and stirs for 1-5 minutes (preferably 2 minutes), then cools and injects into a mold, and cools and shapes to obtain a multi-color lipstick that is easy to adjust.

[0023] Furthermore, in the above application, the multi-color lipstick that is easy to adjust is made of the following raw materials in percentage by mass:

[0024]

[0025]

[0026] Compared with the prior art, the present invention has the following beneficial effects:

[0027] (1) High anthocyanin content: The main coloring substance of cherry pigment is anthocyanin, which is distributed in large quantities in cherry peel and is much higher than the content in the pulp. The present invention uses cellulase to hydrolyze cherry pulp, dissolves the cell wall of the cherry peel, dissolves macromolecular substances, and at the same time reduces the viscosity of the solution, improves the extraction rate of anthocyanin pigments, reduces the difficulty of spray drying, and improves the recovery rate. The present invention uses the response surface method to optimize the key process indicators: enzyme addition amount, enzymatic hydrolysis time and edible ethanol aqueous solution concentration. The optimized scheme increases the anthocyanin content of cherry pigment by 178.59% compared with the traditional method, greatly reducing the loss of raw materials.

[0028] (2) Cherry pigment is currently little studied, and the present invention provides a method basis for the production and application of cherry pigment.

[0029] (3) The present invention applies the prepared cherry pigment to lipstick, which greatly improves the application value of the cherry pigment. Because the cherry pigment prepared by the present invention has a high color value, the proportion of the cherry pigment in the lipstick is only 0.4% at least, which greatly reduces the proportion of the colorant in the lipstick. At the same time, only 1% of the total added pH adjuster is needed to adjust the color of the lipstick in a wide color spectrum of bright red-pink-pink purple, which greatly saves the cost of the colorant and other additives and reduces the research and development cost. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] Figure 1The effects of the amount of cellulase added, enzymatic hydrolysis time and the concentration of edible ethanol aqueous solution on the anthocyanins in cherry pigment powder (the upper part is the contour map, and the lower part is the response surface map);

[0031] Figure 2 The figure shows the obtained cherry pigment powder and its 0.01% added pH 5 aqueous solution. DETAILED DESCRIPTION

[0032] The technical scheme in the embodiment of the present invention is clearly and completely described below, and it is obvious that the described embodiment is only a part of the embodiment of the present invention, rather than all embodiments. Based on the embodiment in the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative work premise belong to the scope of protection of the present invention. The reagent or instrument used in the embodiment of the present invention do not indicate the manufacturer, and are all conventional reagent products that can be obtained by commercial purchase.

[0033] Test method:

[0034] (1) Determination of anthocyanin content: The cherry extract in step (1) or the cherry pigment powder in step (4) is prepared into a solution of a certain concentration, 0.1 mL of the solution is added with 4.9 mL of HCl (pH = 1), shaken well and placed in the dark for 1 h, and the absorbance at wavelengths of 510 nm and 700 nm is measured respectively (A 510 , A 700 ); then take 0.1mL of the extract, add 4.9mL of NaAc-HCl buffer (pH = 4.5), shake well and keep in dark for 50min, and measure the absorbance at 510nm and 700nm wavelengths (A' 510 , A' 700 ); anthocyanin content ρ (mg / 100g) was calculated according to the following formula:

[0035]

[0036] (2) Where: 449.2 is the molar mass of cyanidin-3-O-glucoside (g / mol); 26900 is the molar extinction coefficient of cyanidin-3-O-glucoside; V is the volume of the solution (mL); and N is the dilution factor.

[0037] Example 1

[0038] A method for preparing cherry pigment comprises the following steps:

[0039] (1) Preparation of cherry extract: fresh Mei Zao cherries were washed and pitted, and then crushed with a high-speed grinder to obtain cherry pulp. 100,000 IU of cellulase was added to the cherry pulp at an addition amount of 3 g / 10 kg, and enzymatic hydrolysis was performed in a constant temperature water bath at 45° C. for 5 h. After the enzymatic hydrolysis was completed, the precipitate at the bottom was removed after high-speed centrifugation at 10,000 rpm for 20 min to obtain a cherry extract;

[0040] (2) Macroporous resin extraction: The cherry extract obtained in (1) is subjected to macroporous resin for pigment extraction, and eluted with 30% edible ethanol aqueous solution: After elution, a crude solution of cherry pigment is obtained;

[0041] (3) Concentration: The crude cherry pigment solution obtained in (2) is concentrated under reduced pressure in a water bath at 65° C. and a vacuum degree of −0.08 to −0.1 MPa to obtain a concentrated cherry pigment paste;

[0042] (4) Drying: The obtained cherry pigment concentrated paste is spray-dried to obtain cherry pigment powder. The spray-drying conditions are as follows: an inlet air temperature of 180° C., an outlet air temperature of 90° C., and a flow rate of 10%.

[0043] Example 2-17

[0044] The amount of cellulase added (X3) and the enzymolysis time (X2) in step (1) and the concentration of edible ethanol aqueous solution (X1) in step (2) were adjusted in Example 1. The above three factors were used as influencing factors, and the content of anthocyanin (Y) in cherry pigment powder was used as the response index. The Box-Behnken experiment was performed, and the optimal process index was obtained by optimizing the fitting model through the response surface method, which greatly improved the content of anthocyanin and color value of pigment. The experimental design and results are shown in Table 1, and the one-way analysis of variance (ANOVA) is shown in Table 2.

[0045] Table 1 Box-Behnken experimental design and results

[0046]

[0047]

[0048] Table 2 One-way ANOVA results

[0049]

[0050] Note: * indicates significant difference (0.01<P<0.05); ** indicates extremely significant difference (P<0.01).

[0051] The regression equation obtained by fitting the results obtained from the Box-Behnken experiment with a second-order polynomial is as follows:

[0052] Y=-256.67178+14.30162X1+106.34644X2-9.75933X3-0.840444X1X2+0.254417X1X3+6.77

[0053] 917X2X3-0.138682X1 2 -11.68378X2 2 -5.1115X3 2

[0054] Among them, X1 represents the concentration of edible ethanol aqueous solution (%), X2 represents the enzymolysis time (hours), X3 represents the amount of cellulase added (g / 10kg), and Y represents the content of anthocyanins in cherry pigment powder (mg / 100g). The results of variance analysis showed that the model had a very high significance (P < 0.01), indicating that the model fitting effect was excellent and suitable for subsequent optimization design. The insignificance of the lack of fit term (P > 0.05) further confirmed that the model can fully explain the functional relationship between the influencing factors and the response indicators. X1, X2, X3 and their interaction terms X1X2, X1X3, X2X3, and their respective square terms X12, X22 and X3 2 All of them showed significance, which indicated that these three factors had a significant effect on anthocyanin content, and the influence degree was from large to small, followed by enzymatic hydrolysis time, cellulase addition amount and ethanol concentration. 2 Greater than 0.9, indicating a high correlation between the model and the data. 2 and predict R 2 The difference is less than 0.2, indicating that the regression model can effectively describe the process. In addition, the coefficient of variation CV% is less than 10%, further proving the high reliability and accuracy of the experiment. Based on the above analysis, the model has high fitting accuracy, precision and reliability, and is suitable for further optimization design to determine the best process parameters.

[0055] like Figure 1 The effects of cellulase addition, enzymatic hydrolysis time and edible ethanol aqueous solution concentration on anthocyanins in cherry pigment powder were analyzed. Figure 1As shown in the figure, when the amount of cellulase added is fixed, the anthocyanin content first increases and then decreases with the increase of the concentration of edible ethanol aqueous solution; at a fixed ethanol concentration, the anthocyanin content shows a similar trend with the extension of enzymatic hydrolysis time; and at a fixed enzymatic hydrolysis time, the anthocyanin content also first increases and then decreases with the increase of cellulase addition. Anthocyanins in cherries, such as cyanidin and paeoniflorin, combine with sugar groups to form anthocyanins, which are of various types. The combination of different anthocyanins with sugar groups leads to differences in the polarity of anthocyanins, which affects the elution effect of edible ethanol aqueous solution. Cellulase decomposes cellulose in plant cell walls to produce small molecular sugars. With the increase of enzyme addition, the enzyme activity in cherry slurry is enhanced, which promotes the rupture of cell walls to release anthocyanins on the one hand, and the glucose produced by cellulose decomposition on the other hand increases the possibility of anthocyanin glycosylation to form anthocyanins, thereby increasing the anthocyanin content. However, excessive enzyme addition will cause the generated glucose and cellobiose to inhibit the activity of β-glucanase and β-glucosidase, thereby reducing the anthocyanin content. In addition, too long enzymatic hydrolysis time may lead to partial degradation of anthocyanins due to thermal effects after saturated release, reducing the anthocyanin content.

[0056] When the maximum value of Y is taken as the target, that is, the highest content of anthocyanins in cherry pigment powder is taken as the target, the model is optimized and the optimal process parameters are obtained as follows: 43% concentration of edible alcohol aqueous solution, 4h of enzymatic hydrolysis time, and 3g / 10kg of cellulase addition. At this time, the maximum predicted content of anthocyanins in cherry pigment powder is 235.49mg / 100g.

[0057] Embodiment 18

[0058] A method for preparing cherry pigment comprises the following steps:

[0059] (1) Preparation of cherry extract: fresh Mei Zao cherries were washed and pitted, and then crushed with a grinder at high speed to obtain cherry pulp. 100,000 IU of cellulase was added to the cherry pulp at an addition amount of 3 g / 10 kg, and enzymatic hydrolysis was performed in a constant temperature water bath at 45° C. for 4 h. After the enzymatic hydrolysis was completed, the precipitate at the bottom was removed by high-speed centrifugation at 10,000 rpm for 20 min to obtain a cherry extract;

[0060] (2) Macroporous resin extraction: The cherry extract obtained in (1) is subjected to macroporous resin for pigment extraction, and eluted with 43% edible ethanol aqueous solution: After elution, a crude solution of cherry pigment is obtained;

[0061] (3) Concentration: The crude cherry pigment solution obtained in (2) is concentrated under reduced pressure in a water bath at 65° C. and a vacuum degree of −0.08 to −0.1 MPa to obtain a concentrated cherry pigment paste;

[0062] (4) Drying: The obtained cherry pigment concentrated paste is spray-dried to obtain cherry pigment powder. The spray-drying conditions are as follows: an inlet air temperature of 180° C., an outlet air temperature of 90° C., and a flow rate of 10%.

[0063] The anthocyanin content of the cherry pigment powder was measured and the result was 240.23±1.31 mg / 100 g, which was close to the predicted result. Figure 2 shown.

[0064] Comparative Example 1

[0065] Step (1) in Experimental Example 18 was adjusted as follows: the fresh early cherries were washed and pitted, and the cherries were crushed at high speed using a grinder to obtain cherry pulp. The cherry pulp was centrifuged at 10,000 rpm for 20 min, and the bottom precipitate was removed to obtain a cherry extract.

[0066] The other preparation steps are the same as those in Experimental Example 18.

[0067] Comparative Example 2

[0068] The step (2) in Experimental Example 18 was adjusted as follows: the cherry extract obtained in (1) was subjected to a macroporous resin for pigment extraction, and then eluted with pure water: after elution, a crude solution of cherry pigment was obtained;

[0069] The other preparation steps are the same as those in Experimental Example 18.

[0070] Test Case

[0071] The anthocyanin content and color value of the products of Comparative Example 1 and Comparative Example 2 were measured. The anthocyanin content is shown in Table 1, and the color value content is shown in Table 3

[0072] Table 3 Cherry pigment powder color value measurement results

[0073]

[0074]

[0075] As shown in Table 3, the cherry pigment prepared in Experimental Example 18 has the highest color value, and the color value of cherry pigment prepared in all experimental examples is significantly greater than that of the comparative example. The present invention uses the response surface methodology to optimize key process indicators: enzyme addition amount, enzymolysis time and edible ethanol aqueous solution concentration. The optimized scheme increases the anthocyanin content of cherry pigment by 178.59% compared with the traditional method, greatly reducing the loss of raw materials.

[0076] Embodiment 19

[0077] Table 4 Lipstick formula 1

[0078]

[0079]

[0080] A method for preparing a lipstick that is convenient for color adjustment comprises the following steps:

[0081] S1 weighed cherry pigment and grape seed oil and mixed them, and ground them in a grinder until the liquid was smooth and free of particles;

[0082] S2 weighed water, lecithin, citric acid and sodium citrate, adjusted the pH to 4.4, and stirred in a water bath at 50°C for 20 min;

[0083] S3 heats and melts beeswax, mixes it with the liquid prepared by S1 and S2, heats to 100°C, mixes and stirs for 2 minutes, then cools and injects into a mold, and cools and shapes to obtain a bright red lipstick with L*=41, a*=60, and b*=54.

[0084] Embodiment 20

[0085] Table 5 Lipstick formula 2

[0086] raw material Proportion (%) Cherry pigment prepared in Example 18 0.4 Grapeseed Oil 49 beeswax 20 Lecithin 10 Citric Acid 0.275 Sodium Citrate 0.725 water 19.6

[0087] The preparation steps were the same as those in Example 19, and the pH was adjusted to 5.6 to obtain a reddish-pink lipstick with L*=73, a*=26, and b*=14.

[0088] Embodiment 21

[0089] Table 6 Lipstick formula 3

[0090]

[0091]

[0092] The preparation steps were the same as those in Example 19, and the pH was adjusted to 6.6 to obtain a reddish purple lipstick with L*=52, a*=44, and b*=9.

[0093] As can be seen from the above Examples 19-21, the pH of the product is adjusted by adjusting the content of sodium citrate and citric acid, and the color tone of the cherry pigment in the product is changed. Since the prepared cherry pigment has a high color value, the amount added to the product is only 0.4%, and the amount of the pH adjuster added is only 1%. The proportion of colorants in lipstick is greatly reduced, and the cost of colorants and other additives is greatly saved, reducing R&D costs.

[0094] The above embodiments show and describe the basic principles, main features and advantages of the present invention. Those skilled in the art should understand that the above embodiments do not limit the present invention in any form, and any technical solution obtained by equivalent replacement or equivalent transformation falls within the protection scope of the present invention.

Claims

1. A method for preparing cherry pigment, characterized in that: The following steps are involved: (1) Preparation of cherry extract: fresh cherries are washed and pitted, and then crushed with a grinder at high speed to obtain cherry pulp. Cellulase is added to the cherry pulp and enzymatically hydrolyzed in a constant temperature water bath at 40-50° C. After the enzymatic hydrolysis is completed, the enzymatic hydrolyzate is centrifuged at 8000-12000 rpm for 10-30 minutes, and then the bottom precipitate is removed to obtain the cherry extract; (2) Macroporous resin extraction: The cherry extract obtained in (1) is subjected to a macroporous resin for pigment extraction, and then eluted with an edible ethanol aqueous solution to obtain a crude cherry pigment solution; (3) Concentration: The crude cherry pigment solution obtained in (2) is concentrated under reduced pressure in a water bath at 60-70° C. and a vacuum degree of -0.08 to -0.1 MPa to obtain a concentrated cherry pigment paste; (4) Drying: The obtained cherry pigment concentrated paste is spray-dried to obtain cherry pigment powder.

2. The method for preparing cherry pigment according to claim 1, characterized in that: The cherry used in step (1) is one of Mei Zao, Black Pearl or Red Lantern.

3. The method for preparing cherry pigment according to claim 1, characterized in that: In the step (1), the cellulase activity is 50,000-150,000 IU, the addition amount is 1-5 g / 10 kg, and the enzymolysis time is 2-5 h.

4. The method for preparing cherry pigment according to claim 1, characterized in that: The macroporous resin model in the step (2) is XAD-7.

5. The method for preparing cherry pigment according to claim 1, characterized in that: The concentration of the edible ethanol aqueous solution in step (2) is 30-60% (v / v).

6. The method for preparing cherry pigment according to claim 1, characterized in that: The spray drying conditions in step (4) are as follows: an inlet air temperature of 150-200° C., an outlet air temperature of 80-100° C., and a flow rate of 5-15%.

7. A cherry pigment, characterized in that: The method is prepared by any one of claims 1 to 6.

8. Use of the cherry pigment as claimed in claim 7 in preparing a multi-color lipstick that is convenient for color matching.

9. The use according to claim 8, characterized in that: The preparation method of the lipstick comprises the following steps: S1 Mix cherry pigment and grape seed oil and grind them in a grinder until the liquid is smooth and free of particles; S2 weighs water, lecithin, citric acid and sodium citrate, adjusts the pH to 4.0-7.0, and stirs in a water bath at 40-60°C for 10-30 minutes; S3 heats and melts beeswax, mixes it with the liquid prepared by S1 and S2, heats it to 90-110° C., mixes and stirs for 1-5 minutes, then cools and injects into a mold, and cools and shapes to obtain a multi-color lipstick that is easy to adjust.

10. The use according to claim 9, characterized in that: The multi-color lipstick that is easy to adjust is made of the following raw materials in percentage by mass:

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