CN104856187A - Safe processing method of high antibacterial and antioxidant activity carya cathayensis shell smoking liquid - Google Patents

Safe processing method of high antibacterial and antioxidant activity carya cathayensis shell smoking liquid Download PDF

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Publication number
CN104856187A
CN104856187A CN201510128741.2A CN201510128741A CN104856187A CN 104856187 A CN104856187 A CN 104856187A CN 201510128741 A CN201510128741 A CN 201510128741A CN 104856187 A CN104856187 A CN 104856187A
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smoke solution
pecan shell
high antibacterial
antioxidation activity
product
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CN201510128741.2A
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Chinese (zh)
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王斌
迟长凤
邓尚贵
陈荫
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Zhejiang Ocean University ZJOU
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Zhejiang Ocean University ZJOU
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Priority to CN201510128741.2A priority Critical patent/CN104856187A/en
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Abstract

The present invention discloses a preparing method of high antibacterial and antioxidant activity carya cathayensis shell smoking liquid, and belongs to the technical field of aquatic product processing. The preparing method adopts carya cathayensis shells as a raw material, and includes the following steps: placing the carya cathayensis shells and saccharose in proportion in a distillation apparatus, carrying out dry distillation decomposition and cooling flue gas, thereby obtaining a crude smoking liquid; refining the crude smoking liquid through ethyl acetate, and removing carcinogens with macroporous resin, thereby obtaining the high antibacterial and antioxidation activity carya cathayensis shell smoking liquid. According to the high antibacterial and antioxidation activity carya cathayensis shell smoking liquid, a content of polyphenols is 18.1 to 20.5mg/mL, a content of carbonyl compounds is 9.5 to 10.8 mg/mL, pH value is 2.3 to 2.6, and 3,4 benzopyrene is not detected. The high antibacterial and antioxidation activity carya cathayensis shell smoking liquid can be applied in the aquatic products by atomizing and soaking, has good antibacterial and antioxidant effects, and makes the aquatic product have a rich smoked flavor.

Description

Adopt the processed safely method of the pecan shell smoke solution of high antibacterial antioxidation activity
Technical field
The present invention relates to a kind of preparation method of high antibacterial, antioxidation activity Cigarette made by grain and traditional Chinese medicine Fumeol, be specifically related to adopt that pecan shell wood grain carries out destructive distillation, ethyl acetate is refined and macroreticular resin removes the preparation method of carcinogenic Cigarette made by grain and traditional Chinese medicine Fumeol, belong to technical field of aquatic product processing.
Background technology
Aquatic products sootiness goods, due to the smoked flavor of its uniqueness, are subject to the favor of domestic and international consumer deeply.Adopting the main purpose of sootiness to be the shelf-life extending aquatic product traditionally, now except for except preservation, is more the pursuit to the tempting local flavor of sootiness goods.
The flue gas that tradition fumigating method mainly utilizes the smoulder such as timber, sawdust or imperfect combustion to produce is smoked, aquatic products can be made to lose portion of water and to be able to drying, simultaneously, chemical substance in the flue gas that timber produces and aquatic product produce chemical reaction, make it have corresponding sootiness color and luster and local flavor.Sootiness goods flavor components is mainly derived from the aldehydes matter in flue gas; In the carbonyls of color and luster mainly in flue gas and sootiness goods, protein generation Maillard reaction produced; Secondly, the aldehydes matter in flue gas also has anti-oxidant, sterilization and antisepsis, can holding time of significant prolongation sootiness goods.But existing research shows to be that the compound of representative has certain carcinogenesis with polycyclic aromatic hydrocarbon in flue gas, the danger to human health band; In addition, traditional fumigating method is time-consuming longer, is also unfavorable for the development of sootiness goods industry.Therefore, the traditional fume smoking method of replacement of employing new technology is most important for sootiness industry development.
At present, fumersion technology is subject to extensive concern with its unique advantage.Fumersion method be by smoke solution by flood, spray, smear, the method such as injection joins in raw material, thus the imparting distinctive sootiness fragrance of sootiness goods and color and luster.The aldehydes matter contained in smoke solution, carbonyls etc. and basic simlarity in gas cigarette, most important to the quality of smoke curing quality.In addition, smoke solution is in destructive distillation preparation process, and the carcinogen of representative that a small amount of with polycyclic aromatic hydrocarbon is also retains wherein.Therefore, how to improve the active ingredients such as phenols, and to remove polycyclic aromatic hydrocarbon be the key technology that the carcinogen of representative becomes smoke solution and prepares.
Hickory nut (Carya cathayensis Sarg.), has another name called Juglans mandshurica, juglans mandshurica, main product in China Zhejiang, Anhui have a common boundary the place such as temmoku mountain area, prosperous North.In hickory kernel process, create the fertilizer such as a large amount of pecan shells, be not substantially utilized effectively.The patent No. is the process that the Chinese invention patent of ZL201010535032.3 " utilizes pecan shell to prepare the method for meat fumersion spices " to disclose a kind of extract fumet from pecan shell, is distilled by apricot shell, leaves standstill, the process such as micro-filtration obtains fumersion spices under 300 ~ 550 DEG C of destructive distillation, condensation, normal pressure.Although disclosing of above-mentioned patent utilizes pecan shell to provide the technical scheme of fumersion spices as raw material pyrolysis, but its whole technics comparing is complicated, and active constituent content is lower, especially containing carcinogenic substance 3,4-BaP, is unfavorable for its application in food.
The state of the art of smoke solution is prepared based on the present Research of smoke solution and pecan shell, applicant is that smoke solution prepared by material with pecan shell, and develop rational refining effective ingredients and carcinogenic removing process, obtain a kind of pecan shell smoke solution of high antibacterial, antioxidation activity.
Summary of the invention
Technical problem to be solved by this invention provides that a kind of productive rate is high, bacteriostasis property good for the above-mentioned state of the art, has the walnut shell smoke solution few compared with strong anti-oxidative activity, harmful toxic matter for aquatic products sootiness article treating process, and products obtained therefrom smoked flavor is strong, efficiency-cost ratio good, without the advantage of carcinogenic substance potential hazard, antibacterial favorable anti-corrosion effect.The method adopts refining, the employing macroreticular resin that pecan shell wood grain carries out destructive distillation, employing ethyl acetate carries out high bacteriostatic activity material to remove carcinogenic substance, finally obtain bacteriostasis and contain carcinogenic high-quality food smoke solution by force, not, the content of this smoke solution polyphenols is 18.1 ~ 20.5mg/mL, the content of carbonyl complex is 9.5 ~ 10.8 mg/mL, pH value is 2.3 ~ 2.6, do not detect 3,4-BaP.
The technical scheme that the present invention takes for above-mentioned first technical problem of solution is: a kind of preparation method of pecan shell smoke solution of high antibacterial, antioxidation activity, is characterized in that comprising the following steps:
1) pecan shell pretreatment: select pollution-free, without the pecan shell of mould corruption, removing surface impurity, being crushed to particle diameter is 1 ~ 1.5 cm; According to the ratio of 20:1 to 5:1, pecan shell is mixed with sucrose.
2) the destructive distillation preparation of smoke solution: the sootiness raw material mixed is put into retort 30 ~ 45 min, the section of heating up in a steamer between preparing 300-450 DEG C, decomposes the flue gas produced and collects through serpentine condenser condensation, leave standstill 10 ~ 15h, be rough smoke solution.
3) rough smoke solution is refining: add n-hexane by the rough smoke solution of gained according to the ratio of volume ratio 1:2 ~ 3, and concussion 3 ~ 5 min, leave standstill 10 min, removing n-hexane extract; Remainder adds ethyl acetate according to the ratio of volume ratio 1:3 ~ 5, and concussion 3 ~ 5 min, leave standstill 15 min, obtain ethyl acetate extract, in triplicate, ethyl acetate extract is merged, remove ethyl acetate with Rotary Evaporators in less than 40 DEG C, be refining smoke solution.
4) carcinogenicly to remove: the refining smoke solution of 8 ~ 10 times of column volumes (BV) is joined in pretreated macroporous resin column with the loading speed of 1 ~ 2 mL/min, 6 ~ 9 times of column volume (BV) 95% ethanol are adopted to carry out wash-out with the flow velocity of 1 ~ 3 mL/min, collect eluent, remove 95% ethanol in less than 40 DEG C, obtain the pecan shell smoke solution of high antibacterial, antioxidation activity.
5) package storage: the pecan shell smoke solution of height is antibacterial, antioxidation activity, loads in clean nontoxic brown bottle, sealing, is stored in shady and cool dry place.
As preferably, the pecan shell of step 1) and sucrose ratio (percentage by weight) are 10 ~ 20:1.
Preferred again, the macroreticular resin described in step 4) is XAD-4.
Above-mentioned pecan shell smoke solution that is a kind of high antibacterial, antioxidation activity is used for processing process in aquatic products sootiness goods.The preferred embodiment of the application of described smoke solution in aquatic products smoked products, comprising:
1) smoke solution is formed vaporific by atomising device in the confined space being placed with aquatic products, product is combined with smoke solution, by aeration-drying, smoke solution is combined with product and color development, gives product sootiness color and luster and smoked flavor;
2) product is immersed in the regular hour in smoke solution, product is combined with smoke solution, by aeration-drying, smoke solution is combined with product and color development, gives product sootiness color and luster and smoked flavor;
As preferably, mode 1) in, the time of atomization sootiness is 60 min ~ 90min, different with kind and different according to product form;
As preferably, mode 2) in, the time that product is immersed in smoke solution is 15min ~ 30min, different with kind and different according to product form.
Compared with prior art, the invention has the advantages that:
1, the invention provides a kind of method of higher value application pecan shell, good product effect, the forest resourceies being conducive to improving China utilize, and promote the formation of forestry industrialization.
2, smoke solution preparation method provided by the invention, concise production process environmental protection, production efficiency is high, through fractionation, refining and remove carcinogenic substance and obtain high-quality smoke solution; Product stable effective ingredients, content are high, fungistatic effect is strong, smoke in numerous industry such as product have boundless application space in antibacterial, anticorrosion, preparation.
3, the application mode of smoke solution of the present invention in aquatic product, method is easy, and the product smoked flavor of processing is strong, without carcinogenic substance potential hazard, has good DEVELOPMENT PROSPECT.
Accompanying drawing explanation
Fig. 1 is process chart of the present invention;
The pecan shell smoke solution preparation technology flow chart of the high antibacterial antioxidation activity of Fig. 2.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail.
embodiment:
height is antibacterial, the preparation of the pecan shell smoke solution of antioxidation activity
1) pecan shell pretreatment: select pollution-free, that nothing is mildew and rot pecan shell, removing surface impurity, being crushed to particle diameter is 1.5 cm; According to mass ratio 20:1 to 5:1, pecan shell is mixed with sucrose, the preferred 10:1 of the present embodiment.
2) the destructive distillation preparation of smoke solution: the sootiness raw material mixed is put into retort and decomposes 45 min, the section of heating up in a steamer between preparing 300-450 DEG C, the flue gas of generation is collected through serpentine condenser condensation, leaves standstill 15h, is rough smoke solution.
3) rough smoke solution is refining: add n-hexane by the rough smoke solution of gained according to the ratio of volume ratio 1:2 ~ 3, shake 5 min, leave standstill 10 min, removing n-hexane extract; Remainder adds ethyl acetate according to the ratio of volume ratio 1:3 ~ 5, shakes 5 min, leaves standstill 15 min, obtain ethyl acetate extract, in triplicate, ethyl acetate extract is merged, remove ethyl acetate with Rotary Evaporators in less than 40 DEG C, be refining smoke solution.
4) carcinogenicly to remove: the refining smoke solution of 10 times of column volumes (BV) is joined in pretreated XAD-4 macroporous resin column with 1 mL/min loading speed, 9 times of column volume (BV) 95% ethanol are adopted to carry out wash-out with the flow velocity of 2 mL/min, collect eluent, remove 95% ethanol in less than 40 DEG C, obtain the pecan shell smoke solution of high antibacterial, antioxidation activity.
5) package storage: the pecan shell smoke solution of height is antibacterial, antioxidation activity, loads in clean nontoxic brown bottle, sealing, is stored in shady and cool dry place.
Adopt smoke solution preparation technology of the present invention, the content of the polyphenols that gained height is antibacterial, the pecan shell smoke solution of antioxidation activity adopts Folin-Ciocalteu method to detect is 18.8 mg/mL, the content that hydroxyamine hydrochloride detects carbonyl complex is 10.1 mg/mL, pH value is 2.4, do not detect 3,4-BaP.
pecan shell smoke solution Penaeus Vannmei antibacterial anticorrosion in application
Choose the commercially available fresh Penaeus Vannmei 3 parts of 400g, be placed in the pecan shell smoke solution of 0.5 L 0.3%, Tea Polyphenols and vitamin c solution 25 min respectively, take out draining 5 min, then preserve 10 days under 4 ± 1 DEG C of conditions, detect its total number of bacteria, peroxide value, acid value and VBN (TVB-N value).
The method that the mensuration of acid value and peroxide value specifies with reference to GB/T 5009.37-2003 4.1 is carried out, and the method that the mensuration of TVB-N value specifies with reference to GB/T 5009.44-2003 4.1 is carried out, and the method that total number of bacteria specifies with reference to GB/T 4789.2-2003 is carried out.
Result shows, pecan shell smoke solution is better than Tea Polyphenols under same concentrations and Vc(table 1 in antibacterial, anti-oxidant, anti-aliphatic acid becomes sour and is anticorrosion etc.).
the process of table 1 different solutions is on the impact of Penaeus Vannmei total number of bacteria, peroxide value, acid value and TVB-N value
Pecan shell smoke solution Tea Polyphenols Vitamin C
Total number of bacteria (CFU/g) 3.1×10 5 4.9×10 5 6.8×10 5
Peroxide value (med/100g) 1.72 2.05 2.37
Acid value (mg/g) 1.28 1.55 1.78
TVB-N value (mg/100g) 13.09 15.27 16.98
Finally, still need it is noted that what enumerate above is only two specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be had.All distortion that those of ordinary skill in the art can directly derive from content disclosed by the invention or associate, all should think protection scope of the present invention.

Claims (9)

1. adopt the processed safely method of the pecan shell smoke solution of high antibacterial antioxidation activity, it is characterized in that:
The pecan shell smoke solution of high antibacterial antioxidation activity is adopted to be atomized or immersion treatment aquatic products, to be imbued with product sootiness color and luster and smoked flavor.
2. the processed safely method of the pecan shell smoke solution of the high antibacterial antioxidation activity of employing according to claim 1, is characterized in that: the preparation method of the pecan shell smoke solution of the antibacterial antioxidation activity of described height comprises the steps:
(1) pecan shell pretreatment: select pollution-free, without the pecan shell of mould corruption, removing surface impurity, being crushed to particle diameter is 1 ~ 1.5 cm; In proportion pecan shell is mixed with sucrose;
(2) the destructive distillation preparation of smoke solution: the sootiness raw material mixed is put into retort 30 ~ 45 min, the section of heating up in a steamer between preparing 300-450 DEG C, decomposes the flue gas produced and collects through serpentine condenser condensation, leave standstill 10-15h, be rough smoke solution;
(3) rough smoke solution is refining: add n-hexane by the rough smoke solution of gained according to the ratio of volume ratio 1:2 ~ 3, and concussion 3 ~ 5 min, leave standstill 10 min, removing n-hexane extract; Remainder adds ethyl acetate according to the ratio of volume ratio 1:3 ~ 5, and concussion 3 ~ 5 min, leave standstill 15 min, obtain ethyl acetate extract, in triplicate, ethyl acetate extract is merged, remove ethyl acetate with Rotary Evaporators in less than 40 DEG C, be refining smoke solution;
(4) carcinogenicly to remove: the refining smoke solution of 8 ~ 10 times of column volumes (BV) is joined in pretreated macroporous resin column with 1 ~ 2 mL/min loading speed, 6 ~ 9 times of column volume (BV) 95% ethanol are adopted to carry out wash-out with the flow velocity of 1 ~ 3 mL/min, collect eluent, remove 95% ethanol in less than 40 DEG C, obtain the pecan shell smoke solution of high antibacterial, antioxidation activity.
3. the processed safely method of the pecan shell smoke solution of the high antibacterial antioxidation activity of employing according to claim 2, it is characterized in that: the content that described smoke solution adopts Folin-Ciocalteu method to detect polyphenols is 18.1 ~ 20.5mg/mL, the content that hydroxyamine hydrochloride detects carbonyl complex is 9.5 ~ 10.8 mg/mL, pH value is 2.3 ~ 2.6, do not detect 3,4-BaP.
4. the processed safely method of the pecan shell smoke solution of the high antibacterial antioxidation activity of employing according to claim 3, is characterized in that: in described step (1), pecan shell and sucrose weight percentage are 5 ~ 20:1.
5. the processed safely method of the pecan shell smoke solution of the high antibacterial antioxidation activity of employing according to claim 4, is characterized in that: the macroreticular resin in described step (4) is XAD-4.
6. the processed safely method of the pecan shell smoke solution of the high antibacterial antioxidation activity of employing according to claim 1, it is characterized in that: described atomization processing mode is formed vaporific by smoke solution in the confined space being placed with product by atomising device, product is combined with smoke solution, pass through aeration-drying, smoke solution is combined with product and color development, gives product sootiness color and luster and smoked flavor.
7. the processed safely method of the pecan shell smoke solution of the high antibacterial antioxidation activity of employing according to claim 6, the time that it is characterized in that being atomized in described atomization processing mode sootiness is 60 min ~ 90 min.
8. the processed safely method of the pecan shell smoke solution of the high antibacterial antioxidation activity of employing according to claim 1, it is characterized in that: described immersion treatment mode is for be immersed in the regular hour in smoke solution by product, aquatic products are combined with smoke solution, pass through aeration-drying, smoke solution is combined with product and color development, gives product sootiness color and luster and smoked flavor.
9. the processed safely method of the pecan shell smoke solution of the high antibacterial antioxidation activity of employing according to claim 8, the time that the aquatic products that it is characterized in that in the immersion treatment mode of described application are immersed in smoke solution is 15 min ~ 30 min.
CN201510128741.2A 2015-03-24 2015-03-24 Safe processing method of high antibacterial and antioxidant activity carya cathayensis shell smoking liquid Pending CN104856187A (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106578997A (en) * 2016-12-19 2017-04-26 重庆全航食品有限公司 Preparation method of smoked pig's feet
CN106616437A (en) * 2016-12-19 2017-05-10 重庆全航食品有限公司 Preparation method of smoked beef
CN106879714A (en) * 2017-02-21 2017-06-23 朱军 A kind of preparation method of bowel lavage meat products
CN106912539A (en) * 2017-02-21 2017-07-04 朱军 A kind of preparation method of Luzhou-flavor bowel lavage meat products
CN107668553A (en) * 2017-11-16 2018-02-09 合肥工业大学 A kind of method that meat products is smoked in smoke solution atomization
CN109105459A (en) * 2018-07-19 2019-01-01 浙江瑞邦智能装备股份有限公司 Smoke solution atomization system
CN110959837A (en) * 2019-11-06 2020-04-07 三只松鼠股份有限公司 Preparation method of smoked flavor melon seeds
CN112715907A (en) * 2020-12-23 2021-04-30 河南双汇投资发展股份有限公司 Method for preparing food smoking liquid by using perilla as raw material and application thereof

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CN101999618A (en) * 2010-11-09 2011-04-06 合肥工业大学 Method for preparing liquid smoking spice for meat from pecan shells
CN102805142A (en) * 2012-08-10 2012-12-05 山东东方海洋科技股份有限公司 Preparation method of liquid smoked fish soft cans
CN102836260A (en) * 2012-09-07 2012-12-26 四川大学 Method for extracting plant polyphenol with antioxidant activity from wild pepper leaves
CN104222980A (en) * 2014-07-28 2014-12-24 中国肉类食品综合研究中心 Preparation method and application of fruit tree fumigating liquid

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101999618A (en) * 2010-11-09 2011-04-06 合肥工业大学 Method for preparing liquid smoking spice for meat from pecan shells
CN102805142A (en) * 2012-08-10 2012-12-05 山东东方海洋科技股份有限公司 Preparation method of liquid smoked fish soft cans
CN102836260A (en) * 2012-09-07 2012-12-26 四川大学 Method for extracting plant polyphenol with antioxidant activity from wild pepper leaves
CN104222980A (en) * 2014-07-28 2014-12-24 中国肉类食品综合研究中心 Preparation method and application of fruit tree fumigating liquid

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106578997A (en) * 2016-12-19 2017-04-26 重庆全航食品有限公司 Preparation method of smoked pig's feet
CN106616437A (en) * 2016-12-19 2017-05-10 重庆全航食品有限公司 Preparation method of smoked beef
CN106879714A (en) * 2017-02-21 2017-06-23 朱军 A kind of preparation method of bowel lavage meat products
CN106912539A (en) * 2017-02-21 2017-07-04 朱军 A kind of preparation method of Luzhou-flavor bowel lavage meat products
CN107668553A (en) * 2017-11-16 2018-02-09 合肥工业大学 A kind of method that meat products is smoked in smoke solution atomization
CN109105459A (en) * 2018-07-19 2019-01-01 浙江瑞邦智能装备股份有限公司 Smoke solution atomization system
CN110959837A (en) * 2019-11-06 2020-04-07 三只松鼠股份有限公司 Preparation method of smoked flavor melon seeds
CN112715907A (en) * 2020-12-23 2021-04-30 河南双汇投资发展股份有限公司 Method for preparing food smoking liquid by using perilla as raw material and application thereof

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Application publication date: 20150826