CN102645358B - Preparation method of water-soluble cholesterol lyophilized product derived from serum - Google Patents
Preparation method of water-soluble cholesterol lyophilized product derived from serum Download PDFInfo
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- CN102645358B CN102645358B CN201210099638.6A CN201210099638A CN102645358B CN 102645358 B CN102645358 B CN 102645358B CN 201210099638 A CN201210099638 A CN 201210099638A CN 102645358 B CN102645358 B CN 102645358B
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Abstract
The invention relates to a cholesterol lyophilized product, and in particular relates to a preparation method of a water-soluble cholesterol lyophilized product derived from serum. The preparation method comprises the following steps of: adjusting pH value of the serum to 6.9 by utilizing 1mol/L of sodium hydroxide, taking 150ml of absolute ethyl alcohol for dropwise adding to the continuously stirred serum, stirring the serum for 2h at the room temperature, centrifuging the serum for 10min per 1000g and collecting precipitates; weighing 0.3g of glucan and 6.5g of calcium chloride, dissolving the glucan and the calcium chloride to 500ml of deionized water, dissolving the precipitates collected from the former step by the solution, stirring the solution for 2h at the room temperature, centrifuging the solution for 10min per 1000g and collecting the precipitates again; and redissolving the collected precipitates and lyophilizing the precipitates to obtain a cholesterol- rich lyophilized product. Compared with the prior art, with the adoption of the preparation method, cholesterol is lyophilized and then is redissolved by the deionized water, the appearance is clear and bright, the purity of the cholesterol is high, the repeatability is good, and the recovery rate is high.
Description
[technical field]
The present invention relates to a kind of dried frozen aquatic products of cholesterol, specifically a kind of preparation method of the water-soluble cholesterol dried frozen aquatic products that derives from serum that is applied in biology, medical test research.
[background technology]
Cholesterol, another name cholesterol, chemical formula is C
27h
46o is a kind of steroids and sterol.Cholesterol is water-soluble very poor organic compound, and the solubleness of sterling cholesterol in water approximately only has 0.095mg/L (30 DEG C), therefore, under low like this dissolubility, will be difficult to add as solution preparation or the preparation of calibration object/quality-control product.Contain certain density water-soluble cholesterol owing to having in serum, these water-soluble cholesterol or be combined with some compound, or be combined with lipoprotein, thereby have stronger water-solublely, Given this, some enterprise takes high concentration serum to be used as preparation to use at present, also have some to obtain the cholesterol concentrate of high concentration by concentrated serum, but the defect of these ways is: be difficult to first obtain the product that purity is higher, its serum matrix content is very high, thereby has affected the quality of product; Again, owing to being fluid product, its less stable.
For dry thermal sensitivity goods and need to keep bioactive material, freeze-drying is a kind of effective method.The method has prevented the change of goods physics and chemistry and biological nature effectively, can effectively protect the stability of many thermal sensitivity medicine biological products effective ingredients.Up to the present there are the employing freeze drying process such as a lot of medicines, biological products to be prepared.
[summary of the invention]
The present invention, in order to overcome the deficiencies in the prior art, provides a kind of preparation method of the water-soluble cholesterol dried frozen aquatic products that derives from serum.
To achieve these goals, the present invention has designed a kind of preparation method of the water-soluble cholesterol dried frozen aquatic products that derives from serum, adopts following steps:
A, its pH value is adjusted to 6.9 with the NaOH of 1mol/L, gets in the serum that 150ml absolute ethyl alcohol dropwise adds continuous stirring, after stirring at room temperature 2h, the centrifugal 10min of 1000g, collecting precipitation thing;
B, take 0.3g glucosan and 6.5g lime chloride, be dissolved in 500ml deionized water, by the precipitation of collecting in this solution dissolving step A, after stirring at room temperature 2h, the centrifugal 10min of 1000g, again collecting precipitation thing;
C, the sediment of collecting in step B is dissolved again, freeze-drying afterwards, must be rich in the dried frozen aquatic products of cholesterol.
In described steps A, the content of serum is 1L, and pH is 5-9.
In described step B, the concentration of lime chloride is 25mmol/L.
In described step B, the concentration of glucosan is 2.6mmol/L.
The present invention compared with the existing technology, is redissolved with deionized water after cholesterol freeze-drying, and it is clear and bright that outward appearance is, and cholesterol purity is high, and this dried frozen aquatic products can steady in a long-termly be stored, and method is easy and simple to handle, reproducible, and the recovery is high.And it derives from serum, therefore can be widely used in the field such as biology, medical test.
[embodiment]
The invention provides the dried frozen aquatic products that is rich in water-soluble cholesterol in a kind of serum source.Dried frozen aquatic products good stability provided by the invention, after redissolving, liquid is clear and bright, and or not containing foreign matter or insolubles, water miscible cholesterol neither can not have obvious interference to the detection of conventional project, can not have impact to the stability of other components yet.
Below by embodiment, the invention will be further described.
The present invention is a kind of preparation method of the water-soluble cholesterol dried frozen aquatic products that derives from serum, adopt following steps: (A) taking 1L serum as example, its pH value is adjusted to 6.9 with the NaOH of 1mol/L, get in the serum that 150ml absolute ethyl alcohol dropwise adds continuous stirring, after stirring at room temperature 2h, the centrifugal 10min of 1000g, collecting precipitation thing;
(B) take 0.3g glucosan and 6.5g lime chloride, be dissolved in 500ml deionized water, by the precipitation of collecting in this solution dissolving step A, after stirring at room temperature 2h, the centrifugal 10min of 1000g, again collecting precipitation thing;
(C) sediment of collecting in step B is dissolved again, freeze-drying afterwards, must be rich in the dried frozen aquatic products of cholesterol.
Experiment one, the visual testing of redissolving rear cholesterol
By after the dried frozen aquatic products difference serial number of preparing by above-described embodiment, adopt the table of random numbers to determine the number of draw samples, randomly draw 5 and check.Add deionized water to redissolve, dried frozen aquatic products dissolves fast, and 10-15min dissolves completely, and liquid is clear and bright, not containing foreign matter or insolubles.
The mensuration of experiment two, cholesterol concentration
Cholesterol enzymatic assays is easy, has enough sensitivity, and precision is good, therefore select Determination of Cholesterol By Enzymatic Method concentration.Select Cholesterol Kit, adopt automatic biochemistry analyzer to measure the cholesterol dried frozen aquatic products of 5 redissolution, design parameter sees table.
Known by upper table, the content of cholesterol dried frozen aquatic products is very high.
Experiment three, cholesterol dried frozen aquatic products STABILITY MONITORING
Cholesterol dried frozen aquatic products is placed on to 2-8 DEG C of refrigerator and carries out long-time stability experiment, preserve the concentration by Cholesterol Kit cholesterol detection after the different time, calculate relative deviation, concrete data see table.
Above-mentioned data show, dried frozen aquatic products has good stability.
Claims (1)
1. derive from a preparation method for the water-soluble cholesterol dried frozen aquatic products of serum, adopt following steps:
(A) with the NaOH of 1mol/L, 1L serum pH is adjusted to 6.9, gets in the serum that 150ml absolute ethyl alcohol dropwise adds continuous stirring, after stirring at room temperature 2h, the centrifugal 10min of 1000g, collecting precipitation thing;
(B) take 0.3g glucosan and 6.5g lime chloride, be dissolved in 500ml deionized water, by the precipitation of collecting in this solution dissolving step A, after stirring at room temperature 2h, the centrifugal 10min of 1000g, again collecting precipitation thing;
(C) sediment of collecting in step B is dissolved again, freeze-drying afterwards, must be rich in the dried frozen aquatic products of cholesterol.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210099638.6A CN102645358B (en) | 2012-04-06 | 2012-04-06 | Preparation method of water-soluble cholesterol lyophilized product derived from serum |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210099638.6A CN102645358B (en) | 2012-04-06 | 2012-04-06 | Preparation method of water-soluble cholesterol lyophilized product derived from serum |
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| CN102645358A CN102645358A (en) | 2012-08-22 |
| CN102645358B true CN102645358B (en) | 2014-09-10 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP7110360B2 (en) | 2017-10-09 | 2022-08-01 | テルモ ビーシーティー バイオテクノロジーズ，エルエルシー | Freeze-drying method |
| JP7471316B2 (en) | 2019-03-14 | 2024-04-19 | テルモ ビーシーティー バイオテクノロジーズ，エルエルシー | Multi-part freeze-drying container |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101643495A (en) * | 2009-07-23 | 2010-02-10 | 浙江赞宇科技股份有限公司 | Method for extracting plant sterol from fatty acid or methyl ester distilled black foot thereof |
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2012
- 2012-04-06 CN CN201210099638.6A patent/CN102645358B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101643495A (en) * | 2009-07-23 | 2010-02-10 | 浙江赞宇科技股份有限公司 | Method for extracting plant sterol from fatty acid or methyl ester distilled black foot thereof |
Non-Patent Citations (4)
| Title |
|---|
| 张旭等.蛋黄中胆固醇含量测定方法的研究.《饲料博览》.2011,(第12期),35-38. * |
| 张秀明等.改良荧光法测定血清水溶性脂质过氧化物.《陕西医学检验》.1995,第10卷(第2期),2-4. * |
| 王健等.冷冻干燥对提高脂质体稳定性的研究概况.《中国医药工业杂质》.2005,第36卷576-580. * |
| 黄启平.从羊毛脂中提取胆固醇的研究.《精细化工》.1995,第12卷(第5期),19-20. * |
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Address after: 201100 Shanghai East Road, Minhang District, No. 85 Patentee after: SHANGHAI AILEX TECHNOLOGY Co.,Ltd. Address before: 201100 Shanghai East Road, Minhang District, No. 85 Patentee before: SHANGHAI AILEX TECHNOLOGY Co.,Ltd. |
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Address after: 201108 Lane 152, 468, Beihengsha River Road, Minhang District, Shanghai Patentee after: AILEX TECHNOLOGY GROUP Co.,Ltd. Address before: No. 85 Youdong Road, Minhang District, Shanghai 201100 Patentee before: SHANGHAI AILEX TECHNOLOGY Co.,Ltd. |
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Effective date of registration: 20181211 Address after: 201108 Lane 152, 468, Beihengsha River Road, Minhang District, Shanghai Co-patentee after: ZHEJIANG AILEX MEDICAL Co.,Ltd. Patentee after: AILEX TECHNOLOGY GROUP Co.,Ltd. Address before: 201108 Lane 152, 468, Beihengsha River Road, Minhang District, Shanghai Patentee before: AILEX TECHNOLOGY GROUP Co.,Ltd. |
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