CN102204663B - Tomato sauce added with fennel essential oil - Google Patents
Tomato sauce added with fennel essential oil Download PDFInfo
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- CN102204663B CN102204663B CN2011101161168A CN201110116116A CN102204663B CN 102204663 B CN102204663 B CN 102204663B CN 2011101161168 A CN2011101161168 A CN 2011101161168A CN 201110116116 A CN201110116116 A CN 201110116116A CN 102204663 B CN102204663 B CN 102204663B
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- fennel essential
- tomato sauce
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Abstract
The invention discloses a tomato sauce added with fennel essential oil. Based on weight percentage, the tomato sauce comprises the following ingredients: 15 to 30 percent of tomato paste, 0.1 to 0.25 percent of sodium cellulose glycolate, 5 to 20 percent of cerealose, 0.1 to 5 percent of white granulated sugar, 0.1 to 0.5 percent of xanthan gum, 0.1 to 1 percent of onion powder, 0.2 to 5 percent of common salt, 1.0 to 1.5 percent of fennel essential oil microcapsule, 0.01 to 0.2 percent of clove, 0.1 to 0.5 percent of cassia bark, 0.1 to 1 percent of white pepper, 0.2 to 5 percent of modified starch and the balance being purified water. The preparation method comprises the following steps of: drying, grinding and screening the modified starch seeds to obtain powder; micro-encapsulating the fennel essential oil by the steam distillation method extraction process and the beta-cyclodextrin inclusion method; and performing spice treatment, decoction and mixing, pulping, concentration and filling and sterilization and cooling to obtain the finished product. The tomato sauce is a new tomato sauce variety and has a wide scope of application.
Description
Invention field
The present invention relates to food technology field, concrete, relate to a kind of tomato sauce and preparing technical field thereof that adds the natural antiseptic agent fennel essential oil.
Background technology
Europe fennel (Pimpinella anisum L.), Proterozoic is mostly at Continental Europe and U.S.West Coast.Umbelliferae Foeniculum herbaceos perennial, brightly yellowish look, sowing in spring and autumn, 100 days growth periods, cold-resistant drought-enduring impoverishment tolerant.The special fragrant of tool, the cauline leaf edible, leaf can be mended brain, improves memory, and can be used as the batching of seafood and salad, increases mouthfeel.Seed can be used for the seasonings such as bread, coffee, alec.Can make breath freshening after seed is chewed, help digest and dissolve constipation.Can mix cold dish behind leaf, stem, the germination.Essential oil can be used for making toothpaste, the detoxifcation diuresis of extract tool and the antiobesity action of root, and Turkey is widely used in this Plants in the liquor production.But seed and blade refining are got the liquid deep layer and are stained with clearly skin, use a small amount of essential oil massage muscle, can slow down fatigue.
Food preservative can suppress microbial activities, prevents food apoilage, thereby prolongs the shelf-life of food.Most packaged foods are wanted long preservation, often all will add food preservative.The kind of food preservative is a lot, mainly is divided into synthetic and natural antiseptic agent, and synthetic preservative commonly used is take sorbic acid and salt, benzoic acid and salt and parabens etc. as representative.Synthetic preservative has all passed through a large amount of scientific experiments before going through to use, animal feeding and toxicity toxicological test and evaluation are arranged, and has confirmed can not produce any acute, subacute or chronic hazard to human body.As long as the employed food preservative kind of food production manufacturer, quantity and scope, be strict controlled within the scope that national standard " food additives use sanitary standard " (GB2760-96) stipulates, be can never be hurtful to health, people can relievedly eat.Such as, food seen on market can add the anticorrisive agents such as potassium sorbate, Sodium Benzoate usually, after these two kinds of most widely used anticorrisive agents are taken in by human body, generally can with homaluria, can't accumulate in human body.In China, the anticorrisive agent overwhelming majority who uses in the at present food production is artificial synthetic, and improper use just has certain side effect; Some anticorrisive agent even contain micro-toxin, long-term excessive absorption meeting causes certain infringement to health.Take now widely used food preservative benzoic acid as example, it is used to have dispute in the world always.Such as, because existing benzoic acid and sodium benzoate accumulates long-pending report of poisoning, protection of the child group of the European Community thinks that it should not be used for infant foods, Japan has also made strict restriction to its use.Although, " food additives use sanitary standard " strict regulations the kind of anticorrisive agent, quality standard and additive capacity, numerous food product manufacturing enterprise be subjected to interests order about and in violation of rules and regulations, the illegal phenomenon of abusing, abuse food preservative is very serious.Therefore, in recent years natural antiseptic agent exploitation has become study hotspot, and the anticorrisive agent that must use in some food there is no the report that fennel essential oil is added to tomato sauce research as natural antiseptic agent at present towards safety, nutrition, non-harmful future development.
Summary of the invention
The present invention is directed to prior art and add the present situation technology report of synthetic preservative about tomato sauce, in conjunction with the food processing demand of " green " and " natural ", provide a kind of preparation method of the tomato sauce that adds the natural antiseptic agent fennel essential oil and the tomato sauce of acquisition thereof.
The purpose of this invention is to provide a kind of tomato sauce that adds the natural antiseptic agent fennel essential oil and preparation method thereof.
Purpose of the present invention is achieved through the following technical solutions:
By take fennel as raw material, through and selection full grains, drying, also remove impurity without the fennel seed that goes mouldy; Drying, crushing screening obtain fennel seed powder; Adopt the response surface method to optimize fennel essential oil steam distillation extraction process, set up the multinomial Mathematical Modeling of secondary of extraction of essential oil rate; Analyze derived essential oil by GC-MS, provide the scientific basis of fennel essential oil as natural antiseptic agent and antioxidant application by anti-oxidant, bacteriostatic experiment; The synthetic preservative sodium benzoate that uses with national Specification is determined the optimum dose of fennel essential oil microcapsules as contrast by experiments such as Detection of colony, color difference analysis and subjective appreciations; Can make the fennel flavor tomato sauce that contains the fennel essential oil composition through technical process such as spice processing, infusion allotment, making beating, concentrated can, sterilization coolings.
Particularly, the invention provides a kind of tomato sauce that adds fennel essential oil, its concrete component is according to weight percent meter, and the prescription of the tomato sauce of this fennel essential oil is:
Catsup 15～30%; Sodium carboxymethylcellulose 0.1～0.25%;
Maltose 5～20%; White granulated sugar 0.1～5%;
Xanthans 0.1～0.5%; Onion powder 0.1～1%;
Salt 0.2～5%; Fennel essential oil microcapsules 1.0～1.5%;
Cloves 0.01～0.2% cassia bark 0.1～0.5%
White pepper 0.1～1% converted starch 0.2～5%
Surplus is pure water.
Simultaneously, the invention provides a kind of preparation method who adds the tomato sauce of fennel essential oil, concrete step of preparation process is as follows:
(1) processing of raw material: the fennel seed that selection full grains, drying, nothing are gone mouldy is also removed impurity, drying, pulverize 40 mesh sieves and obtained fennel seed powder, use the steam distillation extraction to obtain essential oil, wherein, the process conditions that steam distillation prepares essential oil of fennel seeds are: power 66W, liquid ratio 6: 1, time 2.5h, recovery rate 4～5%.
(2) preparation of fennel essential oil microcapsules: with pure water and cycloheptaamylose by weight (8～10): 1 mixing makes saturated solution, the fennel essential oil that step (1) is obtained is 1 by weight: ratio (8-10) and this saturated solution mix, at 35～45 ℃ of lower 30～90min that stir, obtain the fennel essential oil microcapsules through vacuum drying.
(3) spice is processed: get cloves, cassia bark, white pepper, add pure water, boil thickening filtration, obtain spice liquid.
(4) infusion allotment: catsup, salt, granulated sugar are put into the double boiler infusion stir, add simultaneously sodium carboxymethylcellulose, xanthans and converted starch; After stirring, add spice liquid.
(5) making beating: the feed liquid after will allocating is put into beater and is pulled an oar, and it is mixed.
(6) concentrated can: the gained feed liquid concentrates, and it is carried out hot filling.
(7) sterilization: carry out 20min sterilization capping at 95 ℃ after the can, then preserve at normal temperatures.
By implementing the concrete summary of the invention of the present invention, can reach following effect:
1. the present invention compared with the prior art, overcome and used synthetic preservative health to be caused the controversial problem of certain infringement, determine and to make an addition in the tomato sauce after the processing of fennel essential oil microcapsules stable state, and provide the suitable amounts of fennel essential oil, not only give the product flavour, and give the product antiseptic effect.
2. for ubiquitous technological difficulties in the prior art, because fennel essential oil highly volatile, must be to its its local flavor of stable state processing competence exertion and preservation, the present invention adopts beta-schardinger dextrin-inclusion method to make the fennel essential oil microencapsulation, and be applied to produce in the tomato sauce, its local flavor conforms to the own nutrient of preservation and tomato sauce and matches, obtain having the tomato sauce of fennel taste, given the product peculiar taste, this is for definite typicalness product provided by the invention, and the tomato sauce that namely adds natural antiseptic agent has important function.
3. the present invention mainly adopts the response surface method to optimize the fennel essential oil extraction process, provide the scientific basis of fennel essential oil as natural antiseptic agent and antioxidant application by anti-oxidant, bacteriostatic experiment, the synthetic preservative sodium benzoate that uses with national Specification is as contrast, determined the optimum dose of fennel essential oil microcapsules by experiments such as Detection of colony, color difference analysis and subjective appreciations, be aided with at last scientific allocation, form fennel flavor tomato sauce simultaneously, give again product certain shelf life.
Description of drawings:
Fig. 1 is shown as the process chart that the tomato sauce of fennel essential oil is added in preparation.
Fig. 2 is shown as the antioxidative activities change curve of fennel essential oil.
Fig. 3 is shown as the antioxidative activities change curve of TBHQ.
Fig. 4 is shown as TBHQ and fennel essential oil is removed the active figure of DPPH.
Fig. 5 is shown as fennel essential oil and removes the active figure of hydroxy radical (OH).
Fig. 6 is shown as TBHQ and removes the active figure of hydroxy radical (OH).
The specific embodiment
Below, for embodiment the present invention is described, still, the present invention is not limited to following embodiment.In addition, in following explanation, if no special instructions, % all refers to the m/m mass percent.
Equipment and material have among the present invention:
The fennel seed is provided by food research and development center, the Central Asia, Xinjiang; Escherichia coli, saccharomycete, aspergillus niger are provided by Microbiological Lab of Xinjiang University; DPPH (1,1-diphenyl-2-picryl hydrazine free radical), ethanol, Phen, hydrogen peroxide, trichloroacetic acid, the potassium ferricyanide, iron chloride, ferrous sulfate, sodium hydrogen phosphate, sodium dihydrogen phosphate, ether, ditert-butylhydro quinone (TBHQ), dimethyl sulfoxide (DMSO), absolute ethyl alcohol, sodium chloride etc. are the A.R. level, nutrient agar, potato culture.
Color difference meter D-25/DP-9000 (U.S. HunterLab company), distillation extraction (SDE) device (the excellent letter electric equipment in Tianzhang City Co., Ltd); GC/MS-QP2010 type gas chromatograph-mass spectrometer (GC-MS) (Japanese SHIMADZU company); HH-S type thermostat water bath (Ying Yu of Gongyi City gives magnificent Co., Ltd); Spectrumlab-53 ultraviolet-visible spectrophotometer (Prism Optical Technology Co); H-1 micro-mixer (upper Haikang standing grain photoelectric instrument Co., Ltd); RE-52AA rotary evaporator (Shanghai Yarong Biochemical Instrument Plant); GNP-9080 water isolation type constant incubator (the upper grand experimental facilities of Nereid Co., Ltd); Clean operating desk (Medical Equipment Plant of Shanghai Boxun Industrial Co., Ltd.); GMSX-280 hand pressure steam sterilizer (Beijing forever bright Medical Instruments factory).
All reagent of selecting among the present invention and instrument all are well known selecting, but do not limit enforcement of the present invention, and other reagent more well known in the art and equipment are all applicable to the enforcement of the following embodiment of the present invention.
Embodiment one: the tomato sauce prescription that adds fennel essential oil
The invention provides a kind of interpolation natural antiseptic agent fennel essential oil tomato sauce, its concrete component is according to weight percent meter, and used prescription is:
Catsup 15%; Sodium carboxymethylcellulose 0.1%;
Maltose 5%; White granulated sugar 0.1%;
Xanthans 0.1%; Onion powder 0.1%;
Salt 0.2%; Fennel essential oil microcapsules 1.0%;
Cloves 0.01% cassia bark 0.1%
White pepper 0.1% converted starch 0.2%
Surplus is pure water.
Embodiment two: the tomato sauce prescription that adds fennel essential oil
The invention provides a kind of interpolation natural antiseptic agent fennel essential oil tomato sauce, its concrete component is according to weight percent meter, and used prescription is:
Catsup 30%; Sodium carboxymethylcellulose 0.25%;
Maltose 20%; White granulated sugar 5%;
Xanthans 0.5%; Onion powder 1%;
Salt 5%; Fennel essential oil microcapsules 1.5%;
Cloves 0.2% cassia bark 0.5%
Surplus is pure water.
Embodiment three: the tomato sauce prescription that adds fennel essential oil
The invention provides a kind of interpolation natural antiseptic agent fennel essential oil tomato sauce, its concrete component is according to weight percent meter, and used prescription is:
Catsup 20%; Sodium carboxymethylcellulose 0.2%;
Maltose 15%; White granulated sugar 2%;
Xanthans 0.3%; Onion powder 0.5%;
Salt 2%; Fennel essential oil microcapsules 1.3%;
Cloves 0.1% cassia bark 0.3%
White pepper 0.5% converted starch 2%
Surplus is pure water.
Embodiment four: add the preparation of fennel essential oil tomato sauce
Referring to accompanying drawing 1
(1) processing of raw material: the fennel seed that selection full grains, drying, nothing are gone mouldy is also removed impurity, drying, pulverize 40 mesh sieves and obtained fennel seed powder, use the steam distillation extraction to obtain essential oil, wherein, the process conditions that steam distillation prepares essential oil of fennel seeds are: power 66W, liquid ratio 6: 1, time 2.5h, recovery rate 4～5%.
(2) preparation of fennel essential oil microcapsules: pure water and cycloheptaamylose are made saturated solution by weight 8: 1 mixings, the fennel essential oil that step (1) is obtained is that ratio and this saturated solution of 1: 8 mixes by weight, at 35 ℃ of lower 30min that stir, obtain the fennel essential oil microcapsules through vacuum drying.
(3) spice is processed: get cloves, cassia bark, white pepper, add pure water, boil thickening filtration, obtain spice liquid.
(4) infusion allotment: catsup, salt, granulated sugar are put into the double boiler infusion stir, add simultaneously sodium carboxymethylcellulose, xanthans and converted starch; After stirring, add spice liquid.
(5) making beating: the feed liquid after will allocating is put into beater and is pulled an oar, and it is mixed.
(6) concentrated can: the gained feed liquid concentrates, and it is carried out hot filling.
(7) sterilization: carry out 20min sterilization capping at 95 ℃ after the can, then preserve at normal temperatures.
Embodiment five: add the preparation of fennel essential oil tomato sauce
(1) processing of raw material: the fennel seed that selection full grains, drying, nothing are gone mouldy is also removed impurity, drying, pulverize 40 sieves and obtained fennel seed powder, use the steam distillation extraction to obtain essential oil, wherein, the process conditions that steam distillation prepares essential oil of fennel seeds are: power 66W, liquid ratio 6: 1, time 2.5h, recovery rate 4～5%.
(2) preparation of fennel essential oil microcapsules: pure water and cycloheptaamylose are made saturated solution by weight 10: 1 mixings, the fennel essential oil that step (1) is obtained is that ratio and this saturated solution of 1: 10 mixes by weight, at 45 ℃ of lower 90min that stir, obtain the fennel essential oil microcapsules through vacuum drying.
(3) spice is processed: get cloves, cassia bark, white pepper, add pure water, boil thickening filtration, obtain spice liquid.
(4) infusion allotment: catsup, salt, granulated sugar are put into the double boiler infusion stir, add simultaneously sodium carboxymethylcellulose, xanthans and converted starch; After stirring, add spice liquid.
(5) making beating: the feed liquid after will allocating is put into beater and is pulled an oar, and it is mixed.
(6) concentrated can: the gained feed liquid concentrates, and it is carried out hot filling.
(7) sterilization: carry out 20min sterilization capping at 95 ℃ after the can, then preserve at normal temperatures.
Embodiment six: add fennel essential oil tomato sauce and preparation thereof
The prescription of the tomato sauce of fennel essential oil is:
Catsup 15～30%; Sodium carboxymethylcellulose 0.1～0.25%;
Maltose 5～20%; White granulated sugar 0.1～5%;
Xanthans 0.1～0.5%; Onion powder 0.1～1%;
Salt 0.2～5%; Fennel essential oil microcapsules 1.0～1.5%;
Cloves 0.01～0.2% cassia bark 0.1～0.5%
White pepper 0.1～1% converted starch 0.2～5%
Surplus is pure water.
(1) processing of raw material: the fennel seed that selection full grains, drying, nothing are gone mouldy is also removed impurity, drying, pulverize 40 mesh sieves and obtained fennel seed powder, use the steam distillation extraction to obtain essential oil, wherein, the process conditions that steam distillation prepares essential oil of fennel seeds are: power 66W, liquid ratio 6: 1, time 2.5h, recovery rate 4～5%.
(2) preparation of fennel essential oil microcapsules: with pure water and cycloheptaamylose by weight (8～10): 1 mixing makes saturated solution, the fennel essential oil that step (1) is obtained is 1 by weight: ratio (8-10) and this saturated solution mix, at 35～45 ℃ of lower 30～90min that stir, obtain the fennel essential oil microcapsules through vacuum drying.
(3) spice is processed: get cloves, cassia bark, white pepper, add pure water, boil thickening filtration, obtain spice liquid.
(4) infusion allotment: catsup, salt, granulated sugar are put into the double boiler infusion stir, add simultaneously sodium carboxymethylcellulose, xanthans and converted starch; After stirring, add spice liquid.
(5) making beating: the feed liquid after will allocating is put into beater and is pulled an oar, and it is mixed.
(6) concentrated can: the gained feed liquid concentrates, and it is carried out hot filling.
(7) sterilization: carry out 20min sterilization capping at 95 ℃ after the can, then preserve at normal temperatures.
More than referring to accompanying drawing 1.
Embodiment seven: the extraction of fennel essential oil
Adopt simultaneously distillation extraction method extraction essential oil of fennel seeds, use the Minitab15.0 DAS, adopt the response surface method of Three factors-levels to optimize fennel essential oil extraction process condition;
1. pre-treatment and material particular diameter
The fennel seed was pulverized 40 mesh sieves through heated-air drying 24h, and sealing normal temperature saves backup.Preliminary experiment is the result show, particle extraction of essential oil when 40 order is effective.Along with particle attenuates, the volatile oil yield increases gradually, but the not obvious even decline of increasing degree behind 40 orders because particle is meticulous, can cause grease chamber or eleocyte too much broken, causes volatile oil to scatter and disappear in crushing process.Therefore experimental raw is got 40 mesh sieve fennel seed powder.
2. steam distillation
Accurately get certain mass fennel seed powder Mg, add deionized water VmL by certain solid-liquid ratio and in the 1000mL distilling flask, place electric jacket to heat certain hour.Directly read the oil reservoir volume.Then water is emitted from instrument outlet, the remainder anhydrous sodium sulfate drying or adopt quick freezing with water freezing after get oil.
3. distillation extraction when essential oil
Accurately take by weighing certain mass fennel seed powder Mg, add deionized water VmL in the 500mL distilling flask by certain solid-liquid ratio, place a simultaneously end of distillation extraction instrument; Get the 80mL ether in the 500mL round-bottomed flask, place the simultaneously other end of distillation extraction instrument, then in the electric jacket of setting power, heat certain hour.After extraction finishes, emit extracted by ether product (extract) from the central exit of abstraction instrument, with extract with anhydrous sodium sulfate drying after rotary evaporation concentrated, namely get fennel essential oil, after the sealing essential oil placed under 4 ℃ of conditions and keeps in Dark Place.
The fennel essential oil recovery rate calculates
Bottle heavy (g) after the extraction of essential oil rate %=[extraction-bottle heavy (g) before extracting]/heavy (g) * 100% of sample
Definite through testing, the optimum process condition that steam distillation prepares essential oil of fennel seeds is: power 66W, liquid ratio 6: 1, time 2.5h, recovery rate are 6.29%.
Embodiment eight: the analysis of fennel essential oil active ingredient
Adopting gaschromatographic mass spectrometry (GC-MS) to analyze fennel essential oil forms;
Form by gas chromatography-mass spectrography technical Analysis fennel essential oil, obtain the total ion current figure that GC-MS analyzes.Qualitative by artificial spectrum analysis and NIST27 and NIST147 library searching, and with the relative mass mark of each composition of area normalization quantitative analysis.
GC condition: RTX-5MS type quartz capillary column (0.25mm * 30mm, 0.25 μ m); Injector temperature is 240 ℃; Heating schedule: since 130 ℃, first with 5 ℃ of min
-1Rise to 240 ℃; Carrier gas is the high-purity helium, presses 96.1kPa before the post, carrier gas flux 1.13m Lmin in the post, and split ratio is 30: 1, sample size 2 μ L.
MS condition: EI ion gun, electron energy 70eV, 200 ℃ of ion source temperatures, 250 ℃ of interface temperature, Multiplier voltage 0.7kV, sweep limits 30～500amu.
Referring to table 1,2 as can be known, the GC-MS analysis result shows that fennel essential oil mainly is comprised of ketone and alkene class, and ketone accounts for 48.86%, and the alkene class accounts for 33.07%, anethole 9.78%.
The essential oil of fennel seeds constituent analysis result that table 1 steam distillation makes
The essential oil of fennel seeds constituent analysis result that table 2 while distillation extraction method makes
Embodiment nine: the non-oxidizability evaluation of fennel essential oil
Antioxidation activity in vitro by antioxidative activities, DPPH clearance rate and hydroxy radical (OH) clearance rate evaluation of measuring fennel essential oil;
1. antioxidative activities is measured
Get the 1mL sample, add the PBS 2.5mL of pH6.6 and 1% six iron cyanogen and close sour potassium solution 2.5mL, place 20min at 50 ℃ after mixing, adding 10% trichloroacetic acid 2.5mL mixes, get mixed liquor 2.5mL, add 2.5mL distilled water and 0.1% ferric chloride solution 2.5mL, leave standstill 10min behind the mixing, measure absorbance (A) at the 700nm place, replace sample as blank absorbance A 0 with reagent.Then TAC can represent with Δ A (Δ A=A-A
0)
The antioxidative activities of essential oil of fennel seeds
Referring to accompanying drawing 2 as can be known, the antioxidative activities of fennel essential oil increases with concentration, and when reaching 10mg/mL, it is maximum that antioxidative activities reaches, and at this moment, concentration increases again, and antioxidative activities descends.Above experimental result explanation, antioxidant is not that concentration is the bigger the better.Because the process that antioxidant (AH) absorbs peroxidating base ROO. generation ROOH and A. is reversible.In high concentration, when temperature raises, the formation speed of polyphenoils free radical (A.) is faster than the speed of substrate autoxidation, when the concentration of antioxidant free radical surpasses peroxide radical or other free radicals, it is the possibility hydroperoxide decomposition just, the result who causes is that antioxidant action descends, even has become prooxidant.When 10mg/mL concentration, the antioxidative activities of fennel essential oil is 0.589; Referring to accompanying drawing 3 as can be known, 10mg/mL concentration fennel essential oil antioxidative activities (0.589) is suitable with the antioxidative activities (0.634) of 0.2mg/mL concentration TBHQ.The research on maximum utilized quantity of TBHQ is 0.2mg/kg (GB2760-1996).
2.DPPH clearance rate is measured
Get the 2mL sample in test tube, then add 2mL
2* 10
-4The DPPH ethanolic solution of mol/L left standstill after shaking up 30 minutes, then calculated clearance rate according to following formula:
Clearance rate %=(Ac-(Ai-Aj)/Ac) * 100
In the formula: Ai: sample liquid and DPPH solution mixed liquor absorbance;
Aj: the absorbance of sample liquid;
Ac:DPPH solution and each are extracted the absorbance of the mixed liquor of reagent.
It is active that fennel essential oil is removed DPPH
Referring to accompanying drawing 4 as can be known, with the increase of concentration, TBHQ and fennel essential oil all increase gradually to the DPPH clearance rate, and fennel essential oil obviously increases.When concentration was 1.2mg/mL, TBHQ was 75.3%, and fennel essential oil is not less than 69.0%, and the two clearance rate is close.
3. hydroxy radical (OH) clearance rate is measured
The phosphoric acid of drawing 4mLpH7.4 is received cushioning liquid, and the Phen that adds 1.5mL5mmol/L is used liquid, fully mixing.Add again the 1mL7.5mmol/L copperas solution, immediately mixing.Add the 1mL sample, immediately mixing.Add the 1.5mL distilled water, to replenish volume.Add at last 0.1% hydrogen peroxide solution, mixing is incubated 1h. in 37 ℃ of water-baths gently, then measures absorbance at the 536nm place.Calculate clearance rate according to following formula.
Clearance rate %=[(A dosing-A damage)/(A does not decrease-the A damage)] * 100
In the formula: the A dosing: add the absorbance that records behind sample and the hydrogen peroxide;
A damage: add hydrogen peroxide and do not add the absorbance of sample;
A does not decrease: the absorbance that records when not adding sample and hydrogen peroxide.
Fennel essential oil is removed hydroxy radical (OH) activity
Referring to accompanying drawing 5 and 6 as can be known, fennel essential oil and TBHQ increase with the increase of concentration hydroxy radical (OH) clearance rate, and fennel essential oil increase than TBHQ significantly.Concentration is the 12mg/mL fennel essential oil to hydroxy radical (OH) clearance rate (78.07%) and concentration is that (83.41%) of 0.2mg/mLTBHQ is suitable.
The fennel essential oil antioxidation activity is remarkable, 10mg/mL concentration fennel essential oil antioxidative activities (0.589) is suitable with the antioxidative activities (0.634) of 0.2mg/mL concentration TBHQ, TBHQ and fennel essential oil are close to DPPH clearance rate ability, and concentration is the 12mg/mL fennel essential oil to hydroxy radical (OH) clearance rate (78.07%) and concentration is that (83.41%) of 0.2mg/mLTBHQ is suitable.
The fennel essential oil antioxidation activity is remarkable
Embodiment ten: the biocidal property research of fennel essential oil
Adopt the filter paper method to analyze the bacteriostatic activity of fennel essential oil;
(1) preparation of bacteria suspension
Preparation culture medium: for subsequent use to the three generations to each bacterial classification inoculation, cellar culture respectively.Get the bacterium stoste after the cultivation, adopt 10 times of dilution methods dilutions, be labeled as successively 10
-1, 10
-2, 10
-3... 10
-8, each concentration is done respectively two parallel laboratory tests.Adopt the method for plate culture count, calculate the bacterium colony of each culture dish after cultivating, getting best is 10 for the examination bacterial concentration
3CFU/mL.
(2) fennel essential oil bacteriostatic experiment
Under aseptic condition, get 10
3Bacteria suspension 0.2mL be coated on the planar surface that solidifies, the bacteria suspension of each concentration do three parallel; Get respectively fennel essential oil solution (the 1mL fennel essential oil mixes with the 1mL dimethyl sulfoxide (DMSO)), 0.2mg/g potassium sorbate solution, 0.2mg/g PhCOONa solution 10mL in the sterilization culture dish, putting into diameter is the neutral filter paper of 8mm, soak 4h, picking up filter paper (by concentration from big to small) with aseptic nipper is attached on the same flat board that the surface contains bacterium clockwise, 37 ℃ of cultivations of bacterium 24h, 28 ℃ of cultivations of saccharomycete 48h, 28 ℃ of cultivations of mould 48h.Cultivate the size of measuring inhibition zone after finishing, calculating mean value.
Minimal inhibitory concentration (MIC) is determined: adopt gradient dilution-flat board to cultivate counting method.Bacterium beef extract-peptone fluid nutrient medium, yeast and aspergillus niger potato fluid nutrient medium.Each tested bacterial classification is got respectively 1mL (10
4Cfu) be inoculated in fluid nutrient medium test tube (3 Duplicate Samples), add respectively volume fraction and be 4.0%, 2.0%, 1.0%, 0.5%, 0.25%, 0.12%, 0.06%, 0.03%, 0.015%, 0.008% and 0.004% anise spirit oil mass, after the homogenizing of vibrating fully, bacterium is in 37 ℃ of cultivation 24h, and yeast and aspergillus niger are cultivated 48h in 30 ℃.Cultivate the existing bacteria growing of test tube explanation of obvious muddiness after finishing, need not to detect again, carry out smearing of nutrition flat board for transparent test tube and cultivate counting, each nutrition flat board respectively drips 0.1mL and treats that test agent cultivates observation, each concentration gradient repeats 3 times, the volume fraction of required essential oil when the minimum antibacterial amount (MIC) of essential oil is defined as original bacterium number reduced 90%.
As seen from the above table, fennel essential oil has significant inhibitory action to mould, and is wherein maximum to the bacteriostasis of aspergillus niger, and saccharomycete, colibacillary bacteriostasis are taken second place, and minimal inhibitory concentration is respectively 0.06%, 0.12% and 1.00%.
Embodiment 11: the preparation of fennel essential oil microcapsules
With water and cycloheptaamylose by weight (8～10): 1 mixing makes saturated solution, to prepare fennel essential oil is 1 by weight: ratio (8-10) and this saturated aqueous solution mix, at 35～45 ℃ of lower 30～90min that stir, obtain the fennel essential oil microcapsules through vacuum drying.
Get the 2g microscapsule powder, add 30mL benzinum mechanical shaking extraction 10min, filter, clean triangular flask and filter residue with the 10mL benzinum again, filtering, at 60 ℃ of lower oven dry 20min, cooling takes by weighing quality, calculates embedding rate.
The theoretical oil content (g) of embedding rate %=[microcapsules-surperficial oil content (g)]/the theoretical oil content (g) * 100% of microcapsules
Adopt the standby fennel essential oil microcapsules of beta-schardinger dextrin-inclusion legal system; The beta-schardinger dextrin-inclusion makes the fennel essential oil microcapsules, and embedding rate is 84.39%.
Embodiment 12: the tomato sauce fresh-keeping effect that adds fennel essential oil is estimated
Interpolation fennel essential oil microcapsules tomato sauce and un-added tomato sauce are placed respectively uncovered cultivation 24h in 37 ℃ of constant incubators, carry out total plate count according to the method for GB4789.2-2010 regulation and measure.
The result shows that the tomato sauce total plate count of adding the fennel essential oil microcapsules is 198/g, and the total plate count of not adding the tomato sauce of fennel essential oil microcapsules is 506/g, illustrates the fennel essential oil microcapsules are added in the tomato sauce that fresh-keeping effect is remarkable.
Embodiment 13: fennel essential oil microcapsules addition is determined
Take aberration, clump count and subjective appreciation as according to determining fennel essential oil microcapsules the suitable addition in tomato sauce suitable with chemical preservative sodium benzoate effect commonly used at present, and for the preparation of fennel flavor tomato sauce.
1. aberration relatively
Aberration represents that with the mode of numerical value two kinds of colors are to the difference on people's color perception with regard to referring to.If two colored samples are all pressed L*, a*, b* demarcates color, then between the two total color difference Δ Eab and each individual event aberration can calculate with following formula: total color difference Δ Eab=[(Δ L*)
2+ (Δ a*)
2+ (Δ b*) 2]
1/2
| ID | L* | a* | b* | C* | Aberration description-rectangle |
| Blank | 99.59 | -0.13 | -0.26 | 0.29 | |
| |
31.65 | 15.59 | 10.35 | 18.71 | Dark, few green, few |
| Tomato sauce | |||||
| 1 reverse side | 31.31 | 15.24 | 10.06 | 18.26 | Dark, few green, few blue |
| The tomato sauce microcapsules are positive | 30.71 | 13.63 | 9.25 | 16.48 | Dark, few green, few blue |
| Tomato sauce microcapsules reverse side | 30.82 | 13.46 | 8.96 | 16.17 | Dark, few green, few blue |
Result:
ID Δ Eab says something
Add the tomato sauce 71.055 of fennel essential oil microcapsules
Tomato sauce 70.641 color and lusters that do not add the fennel essential oil microcapsules are variant
Add the tomato sauce and the Δ Eab=2.284 that does not add the tomato sauce of fennel essential oil microcapsules of fennel essential oil microcapsules, gap is large as can be known by the color difference meter specification, illustrates that the fennel essential oil microcapsules have protective effect to the tomato sauce color and luster.
2. subjective appreciation and clump count
Not only give the product flavour in the tomato sauce with making an addition to after the processing of fennel essential oil microcapsules stable state, and certain antiseptic effect is arranged.The fennel essential oil microcapsules in tomato sauce 1.0～1.5%, optimum addition is 1.3%.
According to the local flavor of fennel itself and the taste compound that determines the sauce local flavor, on the basis of a large amount of exploratory experiments, the synthetic preservative sodium benzoate that employing is used with national Specification is determined the optimum dose of fennel essential oil microcapsules as contrast by methods such as Detection of colony, color difference analysis and subjective appreciations.
Claims (1)
1. tomato sauce that adds fennel essential oil, it is characterized in that, according to weight percent meter, the tomato sauce of this interpolation fennel essential oil contains catsup 15～30%, sodium carboxymethylcellulose 0.1～0.25%, maltose 5～20%, white granulated sugar 0.1～5%, xanthans 0.1～0.5%, onion powder 0.1～1%, salt 0.2～5%, fennel essential oil microcapsules 1.0～1.5%, cloves 0.01～0.2%, cassia bark 0.1～0.5%, white pepper 0.1～1%, converted starch 0.2～5%, surplus is pure water; Wherein, the concrete preparation process of described fennel essential oil microcapsules is as follows:
(1) processing of raw material: the fennel seed that selection full grains, drying, nothing are gone mouldy is also removed impurity, drying, pulverize 40 mesh sieves and obtained fennel seed powder, use the steam distillation extraction to obtain essential oil, wherein, the process conditions that steam distillation prepares essential oil of fennel seeds are: power 66W, liquid ratio 6: 1, time 2.5h, recovery rate 4～5%;
(2) preparation of fennel essential oil microcapsules: with pure water and cycloheptaamylose by weight (8～10): 1 mixing makes saturated solution, the essential oil of fennel seeds that step (1) is obtained is 1 by weight: ratio (8-10) and this saturated solution mix, at 35～45 ℃ of lower 30～90min that stir, obtain the fennel essential oil microcapsules through vacuum drying.
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| CN102669637B (en) * | 2012-05-24 | 2013-09-04 | 石河子天园科技有限公司 | Composite tomato catsup |
| CN103271957A (en) * | 2013-05-25 | 2013-09-04 | 江苏丰园生物技术有限公司 | Fennel oil-mixed cyclodextrin clathrate compound and preparation method thereof |
| CN104273509B (en) * | 2013-07-09 | 2016-08-10 | 普罗旺斯番茄制品（天津）有限公司 | The preparation method of tomato ketchup |
| CN103333741A (en) * | 2013-07-18 | 2013-10-02 | 苏州市天灵中药饮片有限公司 | Preparation method for subcritical fennel essential oil water extraction |
| CN103380890B (en) * | 2013-07-26 | 2014-12-17 | 贵州神奇药物研究院 | Condiment and production method thereof |
| CN103749597B (en) * | 2014-01-02 | 2016-05-25 | 快乐蜂食品（安徽）有限公司 | Special mayonnaise of a kind of baking bread and preparation method thereof |
| CN104187576B (en) * | 2014-07-25 | 2015-08-19 | 统一企业(中国)投资有限公司昆山研究开发中心 | Hygrometric state type catsup flavor pack with fruit feel and preparation method thereof |
| CN104611138A (en) * | 2015-01-30 | 2015-05-13 | 杭州盛华香料有限公司 | Manufacturing process of fennel essence |
| CN104770686A (en) * | 2015-04-20 | 2015-07-15 | 新疆真椒傲农业发展有限公司 | Fennel essence oil shredded pepper and preparation method thereof |
| CN105962306A (en) * | 2016-05-09 | 2016-09-28 | 温州市顶诺食品有限公司 | Black pepper fruit sauce and preparation method thereof |
| CN110907552A (en) * | 2019-12-04 | 2020-03-24 | 中国科学院新疆理化技术研究所 | Method for optimizing supercritical extraction of high-purity fennel essential oil based on response surface method |
| WO2021171320A2 (en) * | 2020-02-24 | 2021-09-02 | Majedifarahani Hedieh | The process of production and formulation of barberry sauce |
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| CN1278625C (en) * | 2004-11-29 | 2006-10-11 | 陈其钢 | A kind of ketchup tomato |
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