阅读说明：本技术 一种外挂式真空冷冻干燥程度的判断方法 (A kind of judgment method of external hanging type vacuum freeze drying degree ) 是由 徐希杰 邹美芬 徐栋 钦晓峰 陆春雄 陈正平 顾晓波 张荣军 俞惠新 张波 李文 于 2019-09-09 设计创作，主要内容包括：本发明涉及一种外挂式真空冷冻干燥程度的判断方法,包括以下步骤：根据待干燥样品的体积选择容器,容器的体积不小于待干燥物品的体积；在容器中加入水,水的体积不小于待干样物品的体积；在容器中加入变色硅胶颗粒；容器中的水和变色硅胶颗粒为指示样品；将指示样品与待干燥样品一起放入到超低温冰箱冷冻,冷冻结束后放入真空冷冻干燥机的外挂罐内；观察变色硅胶颗粒的颜色,变色硅胶颗粒的颜色变为深蓝色时真空冷冻干燥结束。该方法能克服现有目测样品干燥程度主观性判断的缺陷,而提供一种干燥程度的客观判断方法,样品干燥程度的判断效果好,判断的客观性、可信性高,并且更加直观、实用,同时具有提高冻干品质量和减少能耗。(The present invention relates to a kind of judgment methods of external hanging type vacuum freeze drying degree, comprising the following steps: selects container according to the volume of sample to be dried, volume of a container is not less than the volume of article to be dried；Water is added in a reservoir, the volume of water is not less than the volume to dry sample article；Discoloration silica gel particle is added in a reservoir；Water and discoloration silica gel particle in container are instruction sample；Instruction sample and sample to be dried are put into togerther ultra low temperature freezer freezing, are put into after freezing in the outer hanging pot of vacuum freeze drier；The color of observation discoloration silica gel particle, vacuum freeze drying terminates when the color for the silica gel particle that changes colour becomes navy blue.The defect that this method can overcome existing range estimation sample drying degree subjectivity to judge, and provide a kind of objective judgment method of degree of drying, the judgement effect of sample drying degree is good, the objectivity of judgement, credible height, and it is more intuitive, practical, while having and improving dried frozen aquatic products quality and reduction energy consumption.)

1. a kind of judgment method of external hanging type vacuum freeze drying degree, which comprises the following steps:

Container is selected according to the volume of sample to be dried, the volume of a container is not less than the volume of article to be dried；

Water is added in a reservoir, the volume of the water is not less than the volume to dry sample article；

Discoloration silica gel particle is added in a reservoir；

Water and discoloration silica gel particle in the container are instruction sample；

Instruction sample and sample to be dried are put into togerther ultra low temperature freezer freezing, are put into vacuum freeze drying after freezing In the outer hanging pot of machine；

The color of the color of observation discoloration silica gel particle, the discoloration silica gel particle becomes vacuum freeze drying knot when navy blue Beam.

2. a kind of judgment method of external hanging type vacuum freeze drying degree according to claim 1, which is characterized in that

It is weighed and is recorded to container；

It weighs and records after water is added to container, obtain the weight that water is added；

It weighs and records after water and discoloration silica gel particle is added to container；

To samples weighing is indicated when the color of the discoloration silica gel particle becomes navy blue, if weightlessness is not less than addition water at this time Weight then terminates vacuum freeze drying.

3. a kind of judgment method of external hanging type vacuum freeze drying degree according to claim 1, which is characterized in that described Container is transparent vessel.

4. a kind of judgment method of external hanging type vacuum freeze drying degree according to claim 1, which is characterized in that described Cooling time is not less than 12 hours.

5. a kind of judgment method of external hanging type vacuum freeze drying degree according to claim 1, which is characterized in that described The volume of water is 1-1.5 times of the volume of sample to be dried.

6. a kind of judgment method of external hanging type vacuum freeze drying degree according to claim 1, which is characterized in that described Change colour silica gel particle be equipped with it is multiple, the multiple discoloration silica gel particle includes multiple new discoloration silica gel particles or multiple old discoloration silicon The mixing discoloration silica gel particle of one of glue particle or new silica gel particle and old silica gel particle.

7. a kind of judgment method of external hanging type vacuum freeze drying degree according to claim 1, which is characterized in that described Change colour silica gel particle be equipped with it is multiple, the multiple discoloration silica gel particle include the consistent silica gel particle of multiple diameters or mix it is a variety of The discoloration silica gel particle of diameter.

8. a kind of judgment method of external hanging type vacuum freeze drying degree according to claim 6 or 7, which is characterized in that The degree of drying of the multiple discoloration silica gel particle is consistent.

9. a kind of judgment method of external hanging type vacuum freeze drying degree according to claim 1, which is characterized in that described Change colour silica gel particle be equipped with it is multiple, it is the multiple discoloration silica gel particle degree of drying it is consistent.

10. a kind of judgment method of external hanging type vacuum freeze drying degree according to claim 1, which is characterized in that institute The color for stating discoloration silica gel particle becomes continuing after navy blue vacuum refrigeration 0.5-2 hour as the dry further guarantee time.

Technical field

The present invention relates to a kind of judgment methods of the vacuum freeze drying degree of drug, biological sample, especially a kind of outer The judgment method of hanging vacuum freeze drying degree.

Background technique

Vacuum Freezing & Drying Technology is to be now widely used for preparing solid protein pharmaceuticals, oral fast soluble drug and drug The drugs such as embedding medium liposome；Food drying storage；The various fields such as plant dehydration is fresh-keeping.Vacuum freeze drier there are commonly Built-in shelf type and external hanging type, it is built-in to have accurate temperature display system, can accurate judgement sample degree of drying.And it is plug-in Whether formula vacuum freeze drier is only dried with subjective observation judgement sample at present, none more objective judgment criteria. External hanging type vacuum freeze drier does not have more objective judgment criteria as foundation, and the lyophilized technique of sample is just difficult to reach excellent Change.

Summary of the invention

To solve the above problems, the present invention provide it is a kind of can overcome it is existing range estimation sample drying degree subjectivity judge lack It falls into, and provides a kind of objective judgment method of degree of drying, the judgement effect of sample drying degree is good, the objectivity of judgement, can Letter property is high, and more intuitive, practical, while having a kind of external hanging type vacuum refrigeration for improving dried frozen aquatic products quality and reducing energy consumption The judgment method of degree of drying, the specific technical proposal is:

A kind of judgment method of external hanging type vacuum freeze drying degree, comprising the following steps: according to the body of sample to be dried Product selection container, the volume of a container are not less than the volume of article to be dried；Water is added in a reservoir, the volume of the water is not Less than the volume to dry sample article；Discoloration silica gel particle is added in a reservoir；Water and discoloration silica gel particle in the container are Indicate sample；Instruction sample and sample to be dried are put into togerther ultra low temperature freezer freezing, it is cold to be put into vacuum after freezing In the outer hanging pot of lyophilizer；When the color of the color of observation discoloration silica gel particle, the discoloration silica gel particle becomes navy blue Vacuum freeze drying terminates.

By using above-mentioned technical proposal, the water content of vacuum freeze drier sample to be dried usually 98% or more, Avoid containing organic solvent, thereby indicate that the volume of sample water is identical with this or similar, to realize the close of rate of drying, reduced More drying times, energy saving.The weight lost after sample drying to be dried is the moisture lost, therefore will indicate sample In the weight of water that is put into is identical as the weight that dry goods lose that rate of drying can be made close.

The main component of discoloration silica gel is cobalt chloride, and general blue silica gel appearance is blue tinted glass shape particle, in air Water vapour have extremely strong suction-operated, while again can by contained cobalt chloride crystallization water quantity change show different face Color is gradually transformed into light red with the increase of hygroscopic capacity by the blue before moisture absorption.Show the color of moisture approximate content are as follows: deep Blue≤5%, blue≤20%, red=35%, pink >=50%.It is true as external hanging type using this characteristic of discoloration silica gel Vacuum freecing-dry machine judges the indicator of degree of drying, using the characteristic of discoloration silica gel particle dehydration discoloration, color at after dark blue For dry judgment criteria.

Preferably, container is weighed and is recorded；It weighs and records after water is added to container, obtain the weight that water is added Amount；It weighs and records after water and discoloration silica gel particle is added to container；When the color of the discoloration silica gel particle becomes navy blue To instruction samples weighing, terminate vacuum freeze drying if the weightless weight not less than addition water at this time.

By using above-mentioned technical proposal, the weight lost after sample drying to be dried is the moisture lost, therefore will Indicating that the weight for the water being put into sample is identical as the weight that dry goods lose can make rate of drying close.

Preferably, the container is transparent vessel.

By using above-mentioned technical proposal, transparent vessel facilitates the color of observation discoloration silica gel particle.

Preferably, the cooling time is not less than 12 hours.

Preferably, the volume of the water is 1-1.5 times of the volume of sample to be dried.

By using above-mentioned technical proposal, indicate that the weight of sample water can guarantee to do not less than the weight of sample to be dried Dry quality prevents to dry incomplete phenomenon.

The volume of water cannot be more too many greatly than article to be dried, causes drying time elongated too much greatly, and article to be dried is It is completed through dry, and indicates the still unseasoned completion of sample, wasted time and energy consumption.

The discoloration silica gel particle be equipped with it is multiple, the multiple discoloration silica gel particle include multiple new discoloration silica gel particles or The mixing discoloration silica gel particle of one of multiple old discoloration silica gel particles or new silica gel particle and old silica gel particle.

The discoloration silica gel particle be equipped with it is multiple, the multiple discoloration silica gel particle includes the consistent silica gel of multiple diameters The discoloration silica gel particle of grain or mixing multiple diameter.

Preferably, the degree of drying of the multiple discoloration silica gel particle is consistent.

By using above-mentioned technical proposal, degree of drying is consistent with the discoloration discoloration of silica gel particle, to exclude discoloration silicon Glue particle difference leads to not correctly judge drying regime.

Preferably, the discoloration silica gel particle is equipped with multiple, and the degree of drying of the multiple discoloration silica gel particle is consistent.

Preferably, the color of the discoloration silica gel particle continues vacuum refrigeration 0.5-2 hours after becoming navy blue.

By using above-mentioned technical proposal, extension drying time can effectively ensure that dry mass, avoid dry incomplete The phenomenon that.

Compared with prior art the invention has the following advantages:

A kind of judgment method of external hanging type vacuum freeze drying degree provided by the invention can overcome existing range estimation sample dry The defect of dry degree subjectivity judgement, and a kind of objective judgment method of degree of drying is provided, the judgement effect of sample drying degree Fruit is good, the objectivity of judgement, credible height, and more intuitive, practical, while having and improving dried frozen aquatic products quality and reduction energy Consumption, the time control of the vacuum freeze drying suitable for drug, biological sample.

Detailed description of the invention

Fig. 1 is the size and the histogram of drying time of discoloration silica gel particle；

Fig. 2 is the histogram of new discoloration silica gel particle and old discoloration silica gel particle and drying time.

Specific embodiment