CN103919263A - Method for judging freeze drying precooling temperatures of tobacco leaf samples by aid of eutectic crystal points and eutectic melting points - Google Patents
Method for judging freeze drying precooling temperatures of tobacco leaf samples by aid of eutectic crystal points and eutectic melting points Download PDFInfo
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- CN103919263A CN103919263A CN201410140978.8A CN201410140978A CN103919263A CN 103919263 A CN103919263 A CN 103919263A CN 201410140978 A CN201410140978 A CN 201410140978A CN 103919263 A CN103919263 A CN 103919263A
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Abstract
The invention discloses a method for judging freeze drying precooling temperatures of tobacco leaf samples by the aid of eutectic crystal points and eutectic melting points. The method is characterized in that freeze dryers are used as platforms, so that the eutectic crystal points and the eutectic melting points of the fresh tobacco leaf samples in different periods can be measured by the aid of a differential scanning calorimetry (DSC) process, and primary drying temperatures and secondary drying temperatures which are appropriate for fresh tobacco leaf sample freeze drying can be determined. The method has the outstanding advantages that energy-saving and efficient freezing temperatures can be determined on the center of a fresh tobacco leaf vacuum freeze drying process, the appropriate freeze drying process is provided for large quantities of fresh tobacco leaf samples, and accordingly purposes of energy conservation and high efficiency can be achieved.
Description
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Technical field
The present invention relates to vacuum freeze-drying technique, a kind of eutectic point that utilizes specifically, the method of eutectic point judgement tobacco sample freeze drying precooling temperature, that to take VirTis pilot scale type freeze dryer be platform, by poor formula scanning calorimetry (DSC), different times tobacco leaf eutectic point and eutectic point are measured, determine primary drying temperature and redrying temperature that new fresh tobacco leaf freeze drying is comparatively suitable, thereby reach the object of efficient energy-saving.
Background technology
In Plant Metabolome research, generally need to carry out vacuum freeze drying processing to sample, so-called vacuum freeze drying also claims lyophilization, and its principle is that material is freezing, make its moisture containing become ice, then under vacuum, make ice distil and reach drying purpose.Why will carry out vacuum freeze drying to plant sample, this is because (Kim and Verpoorte, 2009): 1) water is enzyme reaction medium, can in sample treatment process, change metabolin and form; 2) water content in different samples is different, to metabolin quantitatively and and then compare to analyze and exert an influence; 3) moisture also can badly influence the resolution ratio of nuclear magnetic resonance (one of metabolism group research important method) spectrum; 4) in freeze drying, enzymatic activity is suppressed by low temperature, and moisture, directly by solid state sublimation, can reduce enzymatic degradation effect greatly.
Moreover in Plant Metabolome research, the general quantity of Plant Metabolome study sample is a lot, a little less is tens parts, is all generally hundreds and thousands of parts, therefore, freeze drying will guarantee that sample metabolism group almost under immovable prerequisite, realizes efficient, energy-conservation object as much as possible.
In freezing dry process, temperature arranges too low, and water sublimed is slower, and freeze-drying needs the time elongated, and Efficiency Decreasing causes energy waste simultaneously; Temperature setting is higher, can make again sample melt, and does not reach the object of vacuum freeze drying.So, find a kind of will but easily method cryodesiccated cryogenic temperature is set just particularly important.Current Freeze Drying Technique is in aspect application such as food processings and report all more (Zhou Guoyan etc., 2010; Pan Qingfang and Zhou Guoyan, 2011; Chun-shan Mountain, pond, 2010), have no the report of its related process research aspect the pretreatment of Plant Metabolome study sample.
Summary of the invention
What object of the present invention provided based on above-mentioned prior art situation just is a kind of simple, determines easily comparatively suitable primary drying temperature and the redrying temperature of new fresh tobacco leaf freeze drying, thereby reaches the object of efficient energy-saving.
The formation mechanism of the inventive method is to utilize two important parameters---eutectic point and eutectic point in vacuum freeze-drying technique, sets up simple, rational freezing method and then reaches energy-efficient object.Eutectic point refers to temperature when moisture fully charge becomes ice crystal in sample, and eutectic point refers to that sample starts the temperature of melting in heating process.
The object of the invention is to be achieved through the following technical solutions:
A kind of eutectic point that utilizes, the method of eutectic point judgement tobacco sample freeze drying precooling temperature, to take freeze dryer as platform, by poor formula scanning calorimetry (DSC), fresh tobacco sample eutectic point and the eutectic point of different times are measured, determined the suitable pre-freeze temperature of fresh tobacco sample freeze drying (pre-freeze temperature is lighted peak dot lower than the eutectic of each sample), primary drying temperature and redrying temperature; Concrete steps are as follows:
(1) get the fresh tobacco sample of different times: cross florescence, transplanting time, squaring period and-80 ℃ of preservation tobacco leaves, used differential scanning calorimeter to measure respectively its heat flow curve;
(2) according to cross florescence, transplanting time, squaring period and-80 ℃ of DSC heat flow curves of preserving tobacco leaf, eutectic point and the eutectic point of four samples are as shown in table 1:
Table 1
| Tobacco sample | Eutectic point (℃) | Eutectic point (℃) |
| The cross florescence | -12.9 | -6.6 |
| Transplanting time | -13.4 | -3.4 |
| Squaring period | -11.5 | -2.9 |
| -80 ℃ of preservations | -9.6 | -1.2 |
(3)according to the eutectic point of record four kinds of tobacco samples and eutectic point data, eutectic point and eutectic point in conjunction with different new fresh tobacco leafs, provide the interval range in eutectic area, congruent melting district, finally determine that freeze dryer is-20 ℃ to the primary drying temperature of tobacco sample, redrying temperature is 0 ℃.
Described freeze dryer is VirTis pilot scale type freeze dryer.
The invention has the advantages that: by poor formula scanning calorimetry (DSC), different times tobacco leaf eutectic point and eutectic point are measured, determine primary drying temperature and redrying temperature that new fresh tobacco leaf freeze drying is comparatively suitable, thereby reached the object of efficient energy-saving.
Accompanying drawing explanation
Fig. 1. the DSC heat flow curve of different fresh tobacco samples.
The specific embodiment
The present invention is described further below in conjunction with accompanying drawing.
Get the fresh tobacco sample of different times (cross florescence, transplanting time, squaring period) and-80 ℃ of preservation tobacco leaves, use differential scanning calorimeter to measure respectively its heat flow curve.Figure 1 shows that cross florescence tobacco leaf and-80 ℃ of DSC heat flow curves of preserving tobacco leaf.Eutectic point and the eutectic point of four samples are as shown in table 1.For saving the energy, improve drying efficiency, in conjunction with eutectic point and the eutectic point of different new fresh tobacco leafs, the primary drying temperature (or claiming eutectic baking temperature) of setting tobacco sample is-20 ℃, redrying temperature (or claiming congruent melting baking temperature) is 0 ℃.
Claims (3)
1. one kind is utilized eutectic point, the method of eutectic point judgement tobacco sample freeze drying precooling temperature, it is characterized in that: be to take freeze dryer as platform, by poor formula scanning calorimetry (DSC), fresh tobacco sample eutectic point and the eutectic point of different times are measured, determined primary drying temperature and redrying temperature that fresh tobacco sample freeze drying is suitable.
2. the eutectic point that utilizes according to claim 1, the method for eutectic point judgement tobacco sample freeze drying precooling temperature, is characterized in that: concrete steps are as follows:
Get the fresh tobacco sample of different times: cross florescence, transplanting time, squaring period and-80 ℃ of preservation tobacco leaves, used differential scanning calorimeter to measure respectively its heat flow curve;
According to cross florescence tobacco leaf, transplanting time, squaring period and-80 ℃ of DSC heat flow curves of preserving tobacco leaf, eutectic point and the eutectic point of four samples are as shown in the table:
According to the eutectic point of record four kinds of tobacco samples and eutectic point data, eutectic point and eutectic point in conjunction with different new fresh tobacco leafs, provide the interval range in eutectic area, congruent melting district, finally determine that freeze dryer is-20 ℃ to the primary drying temperature of tobacco sample, redrying temperature is 0 ℃.
3. the method for utilizing eutectic point, eutectic point judgement tobacco sample freeze drying precooling temperature according to claim 1, is characterized in that: described freeze dryer is VirTis pilot scale type freeze dryer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410140978.8A CN103919263B (en) | 2014-04-10 | 2014-04-10 | One utilizes the method that eutectic point, eutectic point judge tobacco sample lyophilization precooling temperature |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410140978.8A CN103919263B (en) | 2014-04-10 | 2014-04-10 | One utilizes the method that eutectic point, eutectic point judge tobacco sample lyophilization precooling temperature |
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| CN103919263A true CN103919263A (en) | 2014-07-16 |
| CN103919263B CN103919263B (en) | 2016-08-17 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104544541A (en) * | 2014-12-24 | 2015-04-29 | 广西中烟工业有限责任公司 | Preparation method for vacuum freeze drying flower grain electronic cigarette liquid |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB983498A (en) * | 1961-03-18 | 1965-02-17 | Leybold Anlagen Holding Ag | Improvements in or relating to vacuum freeze drying |
| GB1041728A (en) * | 1962-07-24 | 1966-09-07 | Leybold Hochvakuum Anlagen | Improvements in or relating to freeze drying frozen substances, and apparatus therefo |
| CN102511913A (en) * | 2011-12-20 | 2012-06-27 | 红云红河烟草(集团)有限责任公司 | Tobacco shred drying method |
| CN103120359A (en) * | 2013-02-27 | 2013-05-29 | 湖北中烟工业有限责任公司 | Dry method of cigarette tobacco |
| CN103141924A (en) * | 2013-03-26 | 2013-06-12 | 湖北中烟工业有限责任公司 | Tobacco low-temperature drying treatment technology |
-
2014
- 2014-04-10 CN CN201410140978.8A patent/CN103919263B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB983498A (en) * | 1961-03-18 | 1965-02-17 | Leybold Anlagen Holding Ag | Improvements in or relating to vacuum freeze drying |
| GB1041728A (en) * | 1962-07-24 | 1966-09-07 | Leybold Hochvakuum Anlagen | Improvements in or relating to freeze drying frozen substances, and apparatus therefo |
| CN102511913A (en) * | 2011-12-20 | 2012-06-27 | 红云红河烟草(集团)有限责任公司 | Tobacco shred drying method |
| CN103120359A (en) * | 2013-02-27 | 2013-05-29 | 湖北中烟工业有限责任公司 | Dry method of cigarette tobacco |
| CN103141924A (en) * | 2013-03-26 | 2013-06-12 | 湖北中烟工业有限责任公司 | Tobacco low-temperature drying treatment technology |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104544541A (en) * | 2014-12-24 | 2015-04-29 | 广西中烟工业有限责任公司 | Preparation method for vacuum freeze drying flower grain electronic cigarette liquid |
| CN104544541B (en) * | 2014-12-24 | 2016-09-28 | 广西中烟工业有限责任公司 | A kind of preparation method of vacuum lyophilization flower grain electronics ree-oil |
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| CN103919263B (en) | 2016-08-17 |
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