CN1868312A - Process of high speed centrifugal removing lead from bee-glue - Google Patents
Process of high speed centrifugal removing lead from bee-glue Download PDFInfo
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- CN1868312A CN1868312A CNA2005100261680A CN200510026168A CN1868312A CN 1868312 A CN1868312 A CN 1868312A CN A2005100261680 A CNA2005100261680 A CN A2005100261680A CN 200510026168 A CN200510026168 A CN 200510026168A CN 1868312 A CN1868312 A CN 1868312A
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Abstract
A process for removing Pb from propolis by centrifugal method includes such steps as ordinary-temp extracting by alcohol in sealed container, extracting twice in alcohol solution with different concentration, taking supernatant, high-speed centrifugal treating, vacuum concentrating and drying.
Description
Technical field:
The present invention relates to food technology, be specifically related to a kind of propolis and pass through the high speed centrifugation mode new technology of deleading rapidly and efficiently.
Background technology:
To hold be not lead content to content of beary metal in the propolis, is the important indicator of propolis quality, is one of greatest factor of restriction propolis product deep development yet.It is reported that the Brazilian propolis quality of gathering under different regions, the different condition is also different.In the 60t propolis raw material of Japanese import in 1994,92% is that 5% from China from Brazilian import.And 1986-1987 China propolis outlet Japan accounts for larger proportion the lead tolerance of sample is measured, and the result shows: close on metropolitan bee farm, lead tolerance is 2.6-4.5mg/kg in its propolis; Pollution-free area be 1.6-2.0mg/kg; By metal propolis collector adopt for 2.7-3.1mg/kg; That gather on beehive paint top layer is 19.0-52.1mg/kg; The beehive of painting (same bee farm) is not 1.1-2.2mg/kg; Metal surface is 2.5-3.7mg/kg in the beehive; With newspaper pack for 4.9-6.5mg/kg; In the coloured plastics material bag is 3.1-3.6mg/kg.Reports such as the Xu Yun tinkling of pieces of jade in 1989 are once with the propolis sample that covers collection in the same beehive respectively from casing and iron paper money, recording chest portion propolis lead content through atomic absorption spectrophotometry is 6.76mg/kg, the propolis lead content that wire gauze covers collection then far surpasses the content's index that hygiene is permitted, is 38.48mg/kg.Reports such as the calendar year 2001 Guo Jia of China Medical Sciences Academy Medical Plants Institute, to determination of trace element result in the propolis of Beijing, plumbous content is 7.78mg/kg.(place of production: the propolis lead content measurement result of the Tonglu, Hangzhou) carrying out is respectively 32.2mg/kg, 39.85mg/kg to two batches of propolis raw material that the inventor purchased our company in 2002.
Attention degree to lead content is not enough in process of production owing to propolis, cause the 1mg/kg of last gained raw material lead content considerably beyond the national food hygienic standard regulation, and the raw material propolis is not taked the deleading technology, should directly take anything but, and it will bring certain influence to health.
At present deleading mainly contains physics deleading and two kinds of methods of chemical deleading, and wherein chemical deleading method mainly is that (patent No.: 00107422.9): this method is to add 0.02% glacial acetic acid deleading agent to leave standstill and adopt 400 order nylon net filter supernatants to remove metallic lead after 2 hours in ethanol extract by adding deleading agent acetic acid deleading.But the freezing pulverizing of the ingredient requirement of this method, the deleading weak effect is generally less than 10ppm, also can introduce new impurity.Method is in addition filtered neutralisation in addition, absorption method, and the chelating method, but these methods all can be introduced new impurity inevitably.The main method of physics deleading has: (1) supercritical carbon dioxide extraction (patent No.: 99114559.3): though little to the heavy metal meltage with this understanding, generally can be less than 0.2ppm, but the propolis product that extracts yields poorly, Flavonoid substances content is obviously on the low side, and the equipment one-time investment is big.(2) freezing deleading method (patent No.: 00105486.4): pulverize, and variable concentrations edible alcohol (70%, 85%, 95%) is cold soaking repeatedly by liquid nitrogen cryogenics; Freezing sedimentation is 72 hours under-4 ℃ of critical conditions; Add three layer of 80～120 order filter cloth centrifuge and fall filtering lead.This deleading technique requires propolis raw material to need to be crushed to 200 orders through liquid nitrogen cryogenics, and wants three kinds of variable concentrations alcohol to extract repeatedly, subzero 4 ℃ freezing 72 hours ura-rate filtering lead.Can reach 96% though extract yield, the deleading effect can reach below the 0.05ppm, complex process, and the production cycle is long, the cost height.
According to related standards regulation, the lead of the common product of propolis class (as propolis liquid, bee glue soft capsule etc.) limit the quantity of for: fall filtering lead.≤ 0.5mg/kg; General capsule product (propolis hard shell capsules) is :≤1.5mg/kg; Solid (propolis medicinal extract)≤2.0mg/kg.
Therefore, existing propolis deleading technique can not reach the standard code of product.
Summary of the invention:
Technical problem to be solved by this invention is to overcome a kind of propolis deleading technique rapidly and efficiently of above-mentioned weak point design, to obtain to meet the propolis product of food hygiene law regulation lead content standard.
The invention provides a kind of process of high speed centrifugal removing lead from bee-glue, this technology comprises the following steps:
(1) pretreatment of raw material
Propolis raw material is through the freezing fritter of smashing to pieces to 2～3cm;
(2) extraction is centrifugal
Soak under ethanol water normal temperature at following propolis fritter of airtight stirring condition, stirred 30 minutes in per 2 hours, get supernatant aqueous solution high speed centrifugation, time centrifugate of winning and propolis residue, gained propolis residue soaks airtight stirring in 48 hours down through ethanol water normal temperature again, stirred 30 minutes in per 2 hours, and extracted the supernatant high speed centrifugation, get centrifugate and propolis residue for the second time;
(3) vacuum concentrate drying
Twice centrifugate above merging concentrates through 40 ℃～30 ℃ vacuum, and 60 ℃～30 ℃ vacuum drying promptly obtain propolis product.
Step in technology of the present invention (1) cryogenic temperature is 5 ℃～-10 ℃, the weight concentration of step (2) ethanol water is 30～95%, consumption is 1～5 times of propolis weight, and each soak time is that the rotating speed of high speed centrifugation separation in 10～60 hours is 3000～5000rpm.
Process of high speed centrifugal removing lead from bee-glue provided by the invention has following characteristics:
1. generally require low-temperature grinding to less than 40 order requirements to propolis raw material before having simplified the propolis deleading, greatly reduce the expense that preliminary treatment is produced.
2. can guarantee that by this technology propolis extracts yield more than 90%, active ingredient flavones content height.
3. this technology deleading is effective, and the propolis product lead content can reach 0.2～0.05ppm, well below the lead content of state food health legislation regulation.
The specific embodiment:
Embodiment 1.
Propolis raw material is smashed to pieces to the fritter less than 2～3cm through freezing.The propolis fritter was soaked 48 hours airtight stirring (stirring 30 minutes in per 2 hours) down through 3 times of amount 95% alcohol at normal temperature.Get supernatant, (5000rpm) is centrifugal at a high speed, centrifugate and propolis residue.Gained propolis residue soaked 48 hours down through 3 times of amount 75% alcohol at normal temperature, airtight stirring (stirring 30 minutes in per 2 hours).Extract supernatant, high speed centrifugation (5000rpm) gets secondary centrifuging liquid and propolis residue.Twice centrifugate above merging concentrates vacuum drying below 60 ℃ through 40 ℃ of following vacuum.
Embodiment 2.
Propolis raw material is smashed to pieces to the fritter less than 2～3cm through freezing.The propolis fritter was soaked 36 hours airtight stirring (stirring 30 minutes in per 2 hours) down through 4 times of amount 90% alcohol at normal temperature.Get supernatant, high speed centrifugation (4000rpm), centrifugate and propolis residue.Gained propolis residue soaked 48 hours down through 3 times of amount 75% alcohol at normal temperature, airtight stirring (stirring 30 minutes in per 2 hours).Extract supernatant, high speed centrifugation (4000rpm) gets secondary centrifuging liquid and propolis residue.Twice centrifugate above merging concentrates vacuum drying below 60 ℃ through 40 ℃ of following vacuum.
Embodiment 3.
Propolis raw material is smashed to pieces to the fritter less than 2～3cm through freezing.The propolis fritter was soaked 24 hours airtight stirring (stirring 30 minutes in per 2 hours) down through 5 times of amount 85% alcohol at normal temperature.Get supernatant, high speed centrifugation (3000rpm), centrifugate and propolis residue.Gained propolis residue soaked 48 hours down through 3 times of amount 75% alcohol at normal temperature, airtight stirring (stirring 30 minutes in per 2 hours).Extract supernatant, high speed centrifugation (3000rpm) gets secondary centrifuging liquid and propolis residue.Twice centrifugate above merging concentrates vacuum drying below 60 ℃ through 40 ℃ of following vacuum.
Claims (5)
1, a kind of process of high speed centrifugal removing lead from bee-glue is characterized in that this technology comprises the following steps:
(1) pretreatment of raw material
Propolis raw material is smashed to pieces to the fritter less than 2～3cm through freezing;
(2) extraction is centrifugal
Soak under ethanol water normal temperature at following propolis fritter of airtight stirring condition, stirred 30 minutes in per 2 hours, get supernatant aqueous solution high speed centrifugation, time centrifugate of winning and propolis residue, gained propolis residue soaks airtight stirring in 24～48 hours down through alcohol at normal temperature again, stirred 20～40 minutes in per 2 hours, and extracted the supernatant high speed centrifugation, get centrifugate and propolis residue for the second time;
(3) vacuum concentrate drying
Twice centrifugate above merging concentrates through 40 ℃～30 ℃ vacuum, and 60 ℃～30 ℃ vacuum drying promptly obtain propolis product.
, process of high speed centrifugal removing lead from bee-glue according to claim 1, it is characterized in that wherein the described cryogenic temperature of step (1) is 5 ℃～-10 ℃.
3, process of high speed centrifugal removing lead from bee-glue according to claim 1 is characterized in that wherein the weight concentration of the described ethanol water of step (2) is 30～95%, and consumption is 1～5 times of propolis weight.
, process of high speed centrifugal removing lead from bee-glue according to claim 1, it is characterized in that wherein the described soak time of step (2) is each 10～60 hours.
, process of high speed centrifugal removing lead from bee-glue according to claim 1, it is characterized in that wherein the rotating speed of the described centrifugation of step (2) is 3000～6000rpm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2005100261680A CN1868312A (en) | 2005-05-25 | 2005-05-25 | Process of high speed centrifugal removing lead from bee-glue |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2005100261680A CN1868312A (en) | 2005-05-25 | 2005-05-25 | Process of high speed centrifugal removing lead from bee-glue |
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| CN1868312A true CN1868312A (en) | 2006-11-29 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNA2005100261680A Pending CN1868312A (en) | 2005-05-25 | 2005-05-25 | Process of high speed centrifugal removing lead from bee-glue |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102441010A (en) * | 2011-12-12 | 2012-05-09 | 南京中科集团股份有限公司 | Preparation method of deleaded refined propolis |
| CN104721235A (en) * | 2015-04-07 | 2015-06-24 | 北京农科亿健蜂产品研究院 | Producing method of high-quality propolis |
| CN105962356A (en) * | 2016-05-03 | 2016-09-28 | 宣城柏维力生物工程有限公司 | Health-care propolis soft capsules and preparation method thereof |
| CN112826007A (en) * | 2021-01-28 | 2021-05-25 | 北京农科亿健蜂产品研究院 | Device and method for removing heavy metals by propolis mixed liquid |
| CN113926218A (en) * | 2021-11-15 | 2022-01-14 | 老蜂农生物科技集团有限公司 | Production process of propolis ethanol extract and propolis ethanol extract |
-
2005
- 2005-05-25 CN CNA2005100261680A patent/CN1868312A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102441010A (en) * | 2011-12-12 | 2012-05-09 | 南京中科集团股份有限公司 | Preparation method of deleaded refined propolis |
| CN104721235A (en) * | 2015-04-07 | 2015-06-24 | 北京农科亿健蜂产品研究院 | Producing method of high-quality propolis |
| CN105962356A (en) * | 2016-05-03 | 2016-09-28 | 宣城柏维力生物工程有限公司 | Health-care propolis soft capsules and preparation method thereof |
| CN112826007A (en) * | 2021-01-28 | 2021-05-25 | 北京农科亿健蜂产品研究院 | Device and method for removing heavy metals by propolis mixed liquid |
| CN113926218A (en) * | 2021-11-15 | 2022-01-14 | 老蜂农生物科技集团有限公司 | Production process of propolis ethanol extract and propolis ethanol extract |
| CN113926218B (en) * | 2021-11-15 | 2022-12-06 | 老蜂农生物科技集团有限公司 | Production process of propolis ethanol extract and propolis ethanol extract |
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