CN108904753B - Radix curcumae producing area processing technology - Google Patents
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Abstract
The invention provides a radix curcumae producing area processing technology, which comprises the following steps: a. cleaning fresh radix Curcumae, sampling, and steaming for 10-20 min; b. drying: the drying time is 0-30h, and the drying temperature is 45-60 ℃; c. slicing: the slice thickness is 2-8 mm; d. and (3) drying: the drying temperature is 35-75 ℃. The turmeric root tuber decoction pieces prepared by the processing method have better appearance and shape, higher extract and volatile oil content, high curcumin content, accurate and reliable processing method and certain practical value.
Description
Technical Field
The invention relates to a slicing and processing technology of radix curcumae in a producing area.
Background
Curcuma longa L is dried root tuber of Curcuma longa L of Zingiberaceae. The traditional Chinese medicinal material producing area processing is based on the principles of local conditions, simple and convenient operation, simple equipment, low input cost and the like, but the traditional Chinese medicinal material producing area processing often has the defects of long drying period, time and labor waste and the like. The method for processing radix Curcumae in the production area of 2015 edition of Chinese pharmacopoeia comprises collecting and digging after stem and leaf withered in winter, removing silt and fine root, steaming or decocting until it is thoroughly soaked, and drying. Because traditional radix curcumae medicinal material slicing processing needs to pass through the processes of moistening, slicing, drying and the like, a plurality of defects exist, for example, the effective components are lost due to repeated water treatment and drying of the traditional Chinese medicinal materials, the whole processing time is too long, the loss is more, and further the economic benefit is reduced.
Huangwenhua, et al, research on a pressurized infiltration slicing process of radix curcumae, China journal of Chinese medicine, No. 30, No. 7 of 4.2005, which states that the pressurized immersion can significantly shorten the immersion time of medicinal materials, and the pressurized immersion time is related to the short diameter of the cross section of the medicinal materials. The pressurized soaking process comprises soaking at-0.095 MPa for 0.5h, soaking at 0.14MPa for 10-16 h, moistening for 36-48 h, slicing, and air drying at room temperature or oven drying at a temperature not higher than 40 deg.C. Yulan magnolia leaves, et al, the quality of Curcuma longa processed by baking and steaming is compared, the journal of Chinese medicine in the basic level, 1992-07-01, discloses processing Curcuma longa by baking, preferably at 80 ℃.
The existing turmeric root-tuber is mainly produced in places with low channel, high channel, etc. in Sichuan, the processing of medicinal materials is different between the zone with low channel and the zone with high channel, wherein the zone with low channel generally adopts charcoal fire drying, rear collision and collision, and sulfur is contained in coal, which causes the sulfur residue of the medicinal materials to exceed the standard, and part of medical farmers also realize the deficiency, change the modern drying technology into the modern drying technology, but the popularization is not strong, and the method is only limited to a few processing workshops. The method has the advantages that the processing period of the radix curcumae medicinal material is long, the radix curcumae medicinal material is easily influenced by environmental factors, and the phenomenon of mildew is easily caused.
Disclosure of Invention
The technical scheme of the invention is to provide a slicing and processing technology for a producing area of radix curcumae.
The invention provides a radix curcumae producing area processing technology, which comprises the following steps:
a. cleaning fresh radix Curcumae, sampling, and steaming for 10-20 min;
b. drying: the drying time is 0-30h, and the drying temperature is 45-60 ℃;
c. slicing: the slice thickness is 2-8 mm;
d. and (3) drying: the drying temperature is 35-75 ℃.
Wherein the radix curcumae is the turmeric root tuber.
Wherein, the drying time in the step b is 3-9 h.
And c, drying for 4h in the step b.
Wherein, the slicing mode in the step c is as follows: transverse cutting, longitudinal cutting and oblique cutting. Further preferably, the slicing mode is a transverse cutting mode.
Wherein, the slice thickness is 5-6 mm. Further preferably, the slice thickness is 5 mm.
Wherein the drying temperature in the step d is 40-50 ℃. Further preferably, the drying temperature in step d is 43 ℃.
The traditional producing area processing method of the turmeric root-tuber is supplemented and perfected, so that the content of the invention is more scientific and reasonable, the stability and the goodness of the quality of the processed medicinal materials of the turmeric root-tuber producing area are improved and guaranteed, and the economic benefit is further improved and guaranteed.
The turmeric root tuber decoction pieces prepared by the processing method have better appearance and shape, higher extract and volatile oil content, high curcumin content, accurate and reliable processing method and certain practical value.
Obviously, many modifications, substitutions, and variations are possible in light of the above teachings of the invention, without departing from the basic technical spirit of the invention, as defined by the following claims.
The present invention will be described in further detail with reference to the following examples. This should not be understood as limiting the scope of the above-described subject matter of the present invention to the following examples. All the technologies realized based on the above contents of the present invention belong to the scope of the present invention.
Drawings
FIG. 1 is a diagram showing the change of moisture in a sample
FIG. 2 is a graph showing the drying time of a sample before slicing and the measurement result of the quality of the medicinal material
FIG. 3 is a graph showing the measurement results of slicing mode on the quality of medicinal materials
FIG. 4 is a graph showing the measurement results of slice thickness on the quality of medicinal materials
FIG. 5 is a graph showing the results of drying temperature vs. drug substance mass measurement
FIG. 6 is a contour diagram of the slice thickness and the sample drying time before cutting and a 3D response surface diagram (wherein, A. contour line; B. corresponding surface);
FIG. 7 is a contour diagram of drying temperature and sample drying time before cutting and a 3D response surface diagram (wherein, A. contour line; B. corresponding surface);
FIG. 8 is a contour plot of drying temperature versus slice thickness and a 3D response surface plot (wherein A. contour lines; B. corresponding surfaces);
FIG. 9 graph of Curcuma longa sample for response curve experiment
Detailed Description
Example 1 radix Curcumae producing area processing method of the present invention
Materials and instruments
1.1 materials and reagents
Materials: fresh Curcuma longa L.is purchased from Qiancao prefecture in Leshan city of Sichuan province and identified as fresh root tuber of Curcuma longa L.of Zingiberaceae by professor Limin of Chengdu Chinese medicinal university.
Reagent: water was distilled water and methanol was analytically pure. The methanol, the absolute ethyl alcohol and the glacial acetic acid are analytically pure, and the chromatographic acetonitrile and the chromatographic methanol are respectively.
Comparison products: curcumin (batch No. wkq16071501, HPLC ≥ 98%) is provided by Vickers Biotech, Inc. of Sichuan province.
1.2 instruments and devices
Agilent 1200 HPLC (Agilent, usa), far infrared controllable thermoregulation electric heating (sidson electric appliance in sikawa metropolis); DUG-9070B Intelligent electric heating constant temperature air-blast drying oven (Shanghai Lang gan Experimental facilities, Inc.); HX-500A high speed pulverizer for traditional Chinese medicine (Zhejiang Yongkang Xi Chi hardware medical and medical treatment plant); SQP one-thousandth balance (sandoli scientific instruments (beijing) ltd); DZKW-4 electronic constant temperature water bath (Beijing Zhongxing Weiwei instruments Co., Ltd.); KQ-500DE ultrasonic cleaner (ultrasonic instruments Co., Ltd., Kunshan city, Jiangsu province); an SHB-iii S circulating water type multi-purpose vacuum pump (zheng great wall science, industrial and trade, ltd), and the like.
Second, screening process conditions
1. Examination of steaming time
Placing fresh sample in a pan, boiling water, and steaming for 10min, 15min, and 20min respectively. When the turmeric root tuber is steamed for 10min to 15min, the phenomenon of penetration (no hard feeling when the turmeric root tuber is punctured by an iron chisel) is shown. When steaming for 20min, the phenomenon of over-steaming occurs.
And (3) placing the three samples with different processing times in a 50 ℃ oven for drying, wherein the appearance properties of the dried samples are similar.
The results of the determination of the intrinsic component content of the samples at different processing times are shown in table 1.
TABLE 1 influence of different steaming times on herbs
The steaming time of the turmeric does not obviously affect the drying time, but when the turmeric is steamed for 10 minutes, except for low extract content, the volatile oil and curcumin content are highest, and the turmeric is best in quality when the turmeric is steamed for 10 minutes.
2. Investigation of different drying temperatures
And (3) respectively placing the steamed sample for 15 minutes in a blast oven with the temperature of 45 ℃, 50 ℃, 55 ℃ and 60 ℃ for drying, wherein the appearance properties of the obtained sample have no obvious difference at different drying temperatures. The results of comparing the effect of different drying temperatures on the herbs are shown in Table 2.
TABLE 2 results of the effect of different drying temperatures on the quality of the herbs
According to the investigation results of different drying temperatures, the content of the curcuma longa extract increases with the temperature. The content of volatile oil is 50 deg.C highest, 60 deg.C second time, 55 deg.C third time, and 45 deg.C lowest. The curcumin content is optimal at 55 ℃, and the differences of the other three temperatures are not obvious.
3. Research on influence of sample drying time on sample moisture before different cutting
Putting the steamed turmeric sample into an oven for drying, measuring once every 1h, repeating for 3 times, and recording the water content of the sample, wherein the specific conditions are shown in Table 3:
table 3 sample moisture change table (n ═ 3,%)
Note: fresh products are obtained: the water content of the medicinal materials is more than 60 percent; semi-dry product: the water content of the medicinal materials is between 45 and 50 percent; the water content of the dried product is less than 15%.
As can be seen from the figure 1, the sample weight is changed from rapid reduction to slow reduction within 0-30h and finally tends to be stable, the loss condition of the water content of the steamed turmeric in the drying process is reflected, and meanwhile, the turmeric can be confirmed to be dried for 30h, and the water content is basically kept unchanged.
4 Single factor design of experiment
The experiment inspects single-factor operation such as sample drying time before slicing, slicing mode, slicing thickness, drying temperature and the like, influences the contents of water, total ash, extract, volatile oil and curcumin of the curcuma aromatica sample, takes the content of the extract and the content of the curcumin as main objects of inspection, and uses IBM SPSS Statistics 19 software to perform variance difference analysis on data.
4.1 Single factor experiment
4.1.1 study on influence of sample drying time before cutting on quality of medicinal materials
Taking 6 parts of fresh curcuma aromatica, cleaning, steaming, putting into an oven for drying, taking out slices respectively for S1(0H), S2(6H), S3(12H), S4(18H), S5(24H) and S6(30H), cutting into slices in a transverse cutting mode by adopting F1 (transverse cutting), wherein the thickness of the slices is H2(4mm), putting the slices into a W3(55 ℃) oven for drying after cutting, drying to constant weight, measuring the content of components, and comparing the influence of the drying time of a sample before cutting after steaming the curcuma aromatica on the quality of the medicinal materials.
4.1.2 study of the influence of slicing mode on the quality of medicinal materials
Taking 3 parts of the same fresh curcuma aromatica, cleaning, steaming, slicing by respectively adopting F1 (transverse cutting), F2 (longitudinal cutting) and F3 (oblique cutting), wherein the thickness of the slice is H2(4mm), putting the sliced slices into a W3(55 ℃) oven for drying after the slicing is finished, drying to constant weight, and measuring the component content, compared with the influence of the slicing mode of the steamed curcuma aromatica on the quality of the medicinal materials.
4.1.3 study on influence of slice thickness on quality of medicinal materials
Taking 5 parts of fresh curcuma aromatica, cleaning, steaming, respectively slicing by adopting F1 (transverse cutting), controlling the thickness of the decoction pieces to be H1(2mm), H2(4mm), H3(5mm), H4(6mm) and H5(8mm), putting the decoction pieces into a W3(55 ℃) oven for drying after cutting, drying to constant weight, measuring the content of components, and comparing the influence of the thickness of the slices of the steamed curcuma aromatica on the quality of the medicinal materials.
4.1.4 study on the influence of drying temperature on the quality of medicinal materials
Taking 5 parts of fresh curcuma aromatica, cleaning, steaming, slicing by adopting a F1 (transverse cutting) slicing mode, controlling the thickness of the slice to be H2(4mm), putting the slices into W1(35 ℃), W2(45 ℃), W3(55 ℃), W4(65 ℃) and W5(75 ℃) ovens for drying respectively after the slicing is finished, drying to constant weight, measuring the content of components, and comparing the influence of the drying temperature of the steamed curcuma aromatica on the quality of medicinal materials.
4.2 Single factor Experimental results
The results of the determination of water content, total ash content, volatile oil content, extract content and curcumin content are shown in Table 4.
Table 4 measurement results of moisture content, total ash content, and volatile oil content (n ═ 3%)
As can be seen from the table, the moisture content and the total ash content of each treated sample both meet the 2015 edition of Chinese pharmacopoeia. The content range of the volatile oil is 2.00-3.18%.
4.3 analysis of Single-factor Experimental results
4.3.1 influence of sample drying time before slicing on quality of medicinal materials
As can be seen from FIG. 2, the highest values of extract and curcumin contents appeared at 6 h. Through variance analysis, in the similar subsets, significant differences exist among 0h, 6h and 12h in extract content analysis, and significant differences exist among 6h, 0h and 12h in curcumin content analysis, so that 0h, 6h and 12h are selected as horizontal factors.
4.3.2 Effect of slicing mode on medicinal Material quality
As can be seen from FIG. 3, the extract content and curcumin content of the herbs obtained by different slicing methods are in the following order: transverse cutting, oblique cutting and longitudinal cutting; through variance analysis, the extract and curcumin contents of transverse cutting, longitudinal cutting and oblique cutting are significantly different, so the transverse cutting is selected as a slicing mode.
4.3.3 Effect of slice thickness on the quality of medicinal materials
As can be seen from FIG. 4, the highest values of extract and curcumin contents of the sample appeared at 5 mm. Variance analysis shows that the extract content and curcumin content are significantly different among 5mm, 4mm and 6mm, so 4mm, 5mm and 6mm are selected as horizontal factors.
4.3.4 influence of drying temperature on quality of medicinal materials
As can be seen from FIG. 5, the extract and curcumin contents were the highest at 45 ℃; through variance analysis, the contents of extract and curcumin have significant difference between 35 ℃, 45 ℃ and 55 ℃. Therefore, 35 ℃, 45 ℃ and 55 ℃ are selected as horizontal factors.
4.4 nodules
By selecting the data, the response surface experiment design is determined to be 3-factor 3 level, namely: drying time of the sample before cutting: 0h, 6h and 12 h; slice thickness: 4mm, 5mm, 6 mm; drying temperature of the slices: 35 ℃, 45 ℃ and 55 ℃; and (3) adopting a transverse cutting and slicing mode, carrying out response surface design by taking the curcumin content as a response value, and screening the best turmeric producing area slicing processing method. (see FIG. 9)
5-response surface experimental design
On the basis of a single-factor experiment, the drying time, slice thickness and drying temperature of a sample before slicing are selected as influence factors, a slicing mode adopts transverse cutting, Design-Expert8.0.6 software is used for designing according to a Box-Behnken center combination experiment, 15 experimental points and 3 center experimental points are selected, curcumin content is used as a response value, response surface experimental data are analyzed, an optimal experimental operation combination is determined, and further a turmeric producing area slicing processing method is optimized.
5.1 response surface investigation experiment content
Taking 15 parts of the same fresh curcuma aromatica, cleaning, steaming for 30min, penetrating into the core, airing, slicing and drying the sample respectively, wherein the drying time, the slicing thickness and the decoction piece drying temperature of the sample before cutting are shown in tables 5 and 6. X1, X2 and X3 respectively represent the drying time (h), slice thickness (mm) and drying temperature (DEG C) of a sample before cutting, and-1, 0 and 1 respectively represent factor variable levels, the extract and curcumin contents are determined, data analysis processing is carried out by using Design-expert8.0.6 software, the optimal experimental operation combination is determined, and the extract and curcumin contents are reasonably predicted. See table 5, table 6 for details.
TABLE 5 horizontal table for response surface design factor
Table 6 response surface combination design table
5.2 response surface investigation experiment results
The results of the determination of the water content, total ash content, volatile oil, extract and curcumin are shown in Table 7.
Table 7 measurement results of moisture content, total ash content, volatile oil content, extract content, and curcumin content (n ═ 3%)
As can be seen from the table, the contents of the treated water and the total ash content all accord with the Chinese pharmacopoeia of 2015 edition, and the content range of the volatile oil is 2.00-4.00%.
5.3 response surface experiment model establishment and significance test
TABLE 8 design results of response surface analysis
As can be seen from table 8, Design expert8.0.6 software was used to perform quadratic multiple regression fitting on the experimental data to obtain a quadratic multiple regression equation between the sample drying time (a), slice thickness (B), drying temperature (C) and curcumin content (Y) before slicing:
Y2.89-0.034A +0.044B-0.015C-0.037AB +0.065AC-0.050BC-0.11a2-0.072B2-0.13C 2. The model was analyzed for variance and the results are shown in Table 9.
TABLE 9 significance analysis of mathematical models
Mean＝2.73，stddev＝0.060，C.V.＝2.20，R2＝0.9253，R2 adj＝0.7908，R2 pred＝0.4592.
Note: "x" indicates that the difference was extremely significant (P < 0.01); "+" indicates significant difference (P < 0.05)
As can be seen from table 9, the data model was analyzed for variance, and the influence of the sample drying time, slice thickness, and drying temperature on curcumin extraction before slicing was not significant; the secondary terms A2 and C2 have extremely obvious influence on curcumin extraction, B2 has obvious influence on curcumin extraction, and the secondary multivariate terms AB, AC and BC have no obvious influence on curcumin extraction; the P value of the model is less than 0.05, which indicates that the model reaches a significant level and has statistical significance; the F value of the mismatching term is 0.38, the mismatching term is not significant relative to pure error fitting, and the mismatching term is not significant, so that the fitting effect of the equation is better, and the experimental design is scientific and reasonable; (ii) a Meanwhile, the data table shows that the influence sequence of various factors on the determination of the curcumin content is B & gt A & gt C, namely, the slice thickness & gt the sample drying time before cutting & gt the drying temperature.
Regression coefficient R of model20.9253, the correlation between the predicted value and the experimental value of the model is better; coefficient of determination R of model2Adj-0.7908, predicted fitness R2And Pred is 0.4592, which shows that the equation better reflects the relationship between the sample drying time, slice thickness and drying temperature before cutting and the curcumin content, the model fitting degree is better, and the experimental error is smaller. Therefore, the curcumin content determination can be predicted by the model under different operation conditions.
5.4 interaction between variables of response surface experiment
In order to further study the interaction among all factors, regression fitting is carried out on the quadratic multivariate terms AB, AC and BC, and a corresponding response surface and contour map is made, which is shown in figures 6-8. And evaluating the obtained response surface and contour map, and determining the interaction strength among related variables and the optimal range of each variable.
The significance of the interaction between the two variables on the curcumin content of the curcuma aromatica is researched, and a contour map can be analyzed. Determining the significance of the interaction of the two variables according to the curvature value of the corresponding contour map, wherein the larger the curvature is, the more significant the interaction is, namely the flatter the contour line is, the more significant the interaction is, otherwise, the less significant the interaction is; and on the contour diagram, the closer to the outer layer, the lower the extraction content of curcumin, and the closer to the inner layer, the higher the curcumin content.
As shown in fig. 6, the effect of drying temperature and slice thickness on curcumin extraction was investigated when the sample drying time before slicing was fixed at 6 h. As can be seen from the 3D response surface graph, when the sample drying time before slicing is not changed, the extraction of curcumin is in an ascending trend along with the increase of slice thickness, and the ascending trend is slow and slightly reduced after reaching a certain degree; when the slice thickness is constant, the extraction of curcumin tends to increase with the increase of the slice thickness, and tends to decrease after reaching a certain degree. Therefore, the drying time of the sample before cutting is in the range of 3-9h, the slice thickness is fixed in the range of 5-6mm, and the extraction rate of curcumin is highest.
As shown in fig. 7, the effect of the drying time and drying temperature of the sample before slicing on curcumin extraction was investigated when the slice thickness was fixed at 5 mm. As can be seen from the 3D response surface graph, when the sample drying time before cutting is not changed, the extraction of curcumin is in an ascending trend along with the increase of the drying temperature, and is in a descending trend after reaching a certain degree; when the drying temperature is unchanged, the extraction of curcumin is in an upward trend along with the increase of the drying time of the sample before cutting, and is in a downward trend when reaching a certain degree. Therefore, the drying time of the sample before cutting is in the range of 3-9h, the drying temperature is fixed in the range of 40-50 ℃, and the extraction rate of curcumin is highest.
As shown in fig. 8, the effect of slice thickness and sample drying time before slicing on curcumin extraction was investigated when the drying temperature was fixed at 45 ℃. As can be seen from the 3D response surface graph, when the drying temperature is constant, the extraction of curcumin is in an upward trend along with the increase of slice thickness, and when reaching a certain degree, the upward trend is slow and slightly decreased; when the slice thickness is constant, the extraction of curcumin tends to increase with the increase of the drying temperature, and tends to decrease when reaching a certain degree. Therefore, the drying temperature is fixed in the range of 40-50 ℃, the slice thickness is fixed in the range of 5-6mm, and the extraction rate of curcumin is highest.
5.5 determination of optimal extraction Process conditions
Mathematical analysis is carried out on the regression model by using Design-Expert8.06 software, and the optimal method conditions for extracting the curcumin are as follows: the drying time of the sample before cutting is 4.21h, the slicing mode is transverse cutting, the slicing thickness is 5.46mm, the drying temperature is 42.8 ℃, and the extraction of the turmeric root-tuber curcumin can reach 2.9013 mg/g. In consideration of actual operation, the experimental conditions were modified as follows: the drying time of the sample before cutting is 4h, the cutting mode is transverse cutting, the thickness of the cut piece is 5mm, and the drying temperature is 43 ℃.
6 verification experiment
And (3) performing a verification experiment according to the processing method of '5.4', repeating for 2 times, taking the average value of the verification experiment and comparing with a predicted value, and determining the reliability of the slice processing method obtained by utilizing the response surface method for optimization.
6.1 verification of experimental operating results
6.1.1 determination results of moisture, Total Ash, and volatile oil contents
TABLE 10 moisture, Total Ash, volatile oil content scale (%)
6.2 nodules
The experimental result shows that under the condition, the drying time of the sample before cutting is 4h, the cutting mode is transverse cutting, the cutting thickness is 5mm, and the drying temperature is 43 ℃. The extraction of the turmeric root-tuber curcumin reaches 2.8851 mg/g. The error is 0.56% compared to the theoretical prediction. By adopting the response surface method, the optimized extraction method is accurate and reliable and has certain practical value.
7 trait characterization
The sliced curcuma aromatica is dried in different treatment modes, the shape characteristics, the skin characteristics, the section characteristics, the texture and the smell of the sliced curcuma aromatica are observed, and the shape characteristic difference among samples is found to be small, so the sliced curcuma aromatica is subjected to overall analysis. The turmeric root tuber decoction pieces are round, the wrinkles of the skin are obvious, and the turmeric root tuber decoction pieces are brownish gray or grayish yellow; the section is in a cutin shape, the periphery is brown yellow or brown red, and the middle part is light yellow; the texture is hard, the steel wire is not easy to break, and the sound is crisp and loud when the steel wire is broken; light smell, pungent and spicy taste.
8 conclusion and discussion
The experiment inspects the influence of the drying time, the slicing mode, the slicing thickness and the drying temperature of the sample before cutting on the curcumin extraction in the curcuma aromatica by a response surface method. According to the significance analysis of the mathematical model, the model regression difference of the quadratic equation is extremely significant, the F value of the mismatching term is 0.38, the mismatching term is not significant relative to the pure error fitting, the mismatching term is not significant, the fitting effect of the equation is better, and the experimental design is scientific and reasonable; (ii) a Meanwhile, the data table shows that the influence sequence of various factors on the determination of the curcumin content is B & gt A & gt C, namely, the slice thickness & gt the sample drying time before cutting & gt the drying temperature.
The best method for processing the sliced curcuma aromatica in the producing area comprises the following steps: collecting fresh curcuma aromatica, cleaning, sampling and steaming, wherein the processing conditions are as follows: the drying time of the sample before cutting is 4h, the cutting mode is transverse cutting, the thickness of the cut piece is 5mm, and the drying temperature is 43 ℃. The processing method is accurate and reliable by adopting a response surface method, and has certain practical value.
Claims (4)
1. A processing technology of radix curcumae in producing area is characterized in that: it comprises the following steps:
a. cleaning fresh radix Curcumae, sampling, and steaming for 10-15 min;
b. drying: the drying time is 3-9h, and the drying temperature is 45-60 ℃;
c. slicing: the slice thickness is 5-6 mm;
d. and (3) drying: the drying temperature is 40-50 ℃;
the radix curcumae is the turmeric root tuber;
the slicing mode in the step c is as follows: and (4) transverse cutting.
2. The process of claim 1, wherein: and b, drying for 4 h.
3. The process of claim 1, wherein: the slice thickness is 5 mm.
4. The process of claim 1, wherein: and d, the drying temperature is 43 ℃.
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