CN103315956B - A kind of mustard oil nano-emulsion and preparation method thereof - Google Patents
A kind of mustard oil nano-emulsion and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of mustard oil nano-emulsion and preparation method thereof.In nano-emulsion of the present invention, primary surfactant is the mixture of the one or more than one in polyoxyethylene hydrogenated Oleum Ricini RH40, lecithin, poloxamer; Oil phase is mustard oil or the oleic acid solutions being dissolved with mustard oil.Its mass percent consists of: surfactant accounts for 1.38% ~ 22.5% mutually, and oil phase accounts for 0.196% ~ 2.63%, and aqueous phase accounts for 75% ~ 98.4%.Its preparation method is first proportionally mixed homogeneously with cosurfactant by primary surfactant, then adds mustard oil or be dissolved with the oleic acid solutions of mustard oil and ultrasonic disperse, adds ultra-pure water, obtain mustard oil oil-in-water type nano-emulsion in its mixture the most backward.Mustard oil nano-emulsion prepared by the present invention improves the penetrating odor of mustard oil, avoids the volatilization of mustard oil, can food and medicine antibacterial on be applied.
Description
Technical field
The invention belongs to food, medical art, relate to a kind of mustard oil nano-emulsion and preparation method thereof.
Background technology
Mustard oil originates in China, a kind of flavored oils got through squeezing with black mustard or Semen Sinapis Albae, and its main component is allyl isosulfocyanate (AITC).Mustard oil can the secretion of saliva stimulating and gastric juice, has the effect of appetizing, can appetite strengthening.Mustard oil has very strong function of detoxification, can separate the poison of fish Eriocheir sinensis, therefore eats the seafoods such as salmon fish raw and often can mix mustard.Mustard oil not only can prevent decayed tooth, to prophylaxis of cancer, prevents vascular clot, and treatment asthma waits also has certain effect.Mustard oil prevents the effect such as hyperlipidemia, hypertension, heart disease, minimizing blood viscosity in addition.Mustard oil has effect of looks improving and the skin nourishing, and on beauty treatment circle, mustard oil is good massage oil.Mustard oil also has anticancer, antibacterial antiseptical effect simultaneously.
But mustard oil pungent is strong, and pure mustard oil often can stimulate human eye to shed tears, mustard oil volatility is extremely strong simultaneously, unsuitable long-term storage.In real life, the application of mustard oil is limited by very large.In order to solve the above-mentioned defect of mustard oil, adopting the technology of microemulsion, effectively can improve their using value.
Microemulsion be one be made up of water, oil and amphiphilic material, optically stable on isotropy, thermodynamics solution system.This dispersion has the features such as decentralized photo particle particle diameter little (10 ~ 100nm), ultralow interfacial tension, solubilizing amount are large, Thermodynamically stable.Since chemist Hoar and Schulman proposes the concept of microemulsion, cause the interest of increasing people to microemulsion.
Summary of the invention
Technical problem to be solved by this invention is stability in order to improve mustard oil and reduces zest, mustard oil nano-emulsion providing a kind of oil-in-water type and preparation method thereof.
Mustard oil nano-emulsion of the present invention is made up of surfactant phase, oil phase and aqueous phase, its mass percent consists of: surfactant accounts for 1.38% ~ 22.5% mutually, oil phase accounts for 0.196% ~ 2.63%, aqueous phase accounts for 75% ~ 98.4%, wherein surfactant comprises primary surfactant and cosurfactant mutually, the mass ratio of primary surfactant and cosurfactant is 3:1 ~ 1:1, and oil phase is mustard oil or the oleic acid solutions being dissolved with mustard oil.
Above-mentioned mustard oil nano-emulsion preparation method comprises the following steps:
(1) preparation of surfactant
By primary surfactant in 50 ~ 60 DEG C of heating 30 ~ 60 minutes, it is made to become thick liquid by paste; Add cosurfactant again to stir, pack;
(2) preparation of the oleic acid solutions of mustard oil
Under room temperature, mustard oil is joined in oleic acid, shake up to transparence, have no obvious two phase stratification phenomenon, stand-by;
(3) directly by mustard oil or in the oleic acid solutions being dissolved with mustard oil prepared in step (2) being joined surfactant that step (1) prepares, ultrasonic disperse 1 ~ 3 time, each 3 ~ 5 minutes, at every turn ultrasonic interval was 2 ~ 5 minutes;
(4) add ultra-pure water in the system obtained to step (3) with constant flow pump, stir on magnetic stirring apparatus, constant flow pump flow velocity is set to 0.8 ~ 2.0ml/min, and agitator speed is set to 400 ~ 600r/min, can obtain the nano-emulsion of blue-tinted transparent shape simultaneously.
Described primary surfactant is selected from the mixture of the one or more than one in polyethylene glycol hydrogenated Semen Ricini RH40, lecithin or poloxamer; Described cosurfactant is selected from the mixture of the one or more than one in ethanol, propanol, isopropyl alcohol, n-butyl alcohol or isobutanol.
In described mustard oil nano-emulsion, the content of mustard oil is 2mg/ml ~ 20mg/ml.This nano-emulsion can be diluted by ultra-pure water.
Preparation-obtained mustard oil nano-emulsion particle diameter is 13.36 ~ 246.5nm.
Described mustard oil nano-emulsion all has good antibacterial effect to penicillium sp and aspergillus niger, and its inhibition zone size is respectively 2.5 ~ 7.4mm and 3.2 ~ 9.1mm.
Outstanding feature of the present invention and beneficial effect are:
1, it is little that the mustard oil nano-emulsion that prepared by the present invention has particle diameter, the feature of even particle size distribution.Ratio with mustard oil active in effects on surface, add the content of mustard oil and add the isoparametric control of amount of ultra-pure water, the mustard oil nano-emulsion of variable concentrations can be obtained.
2, preparation method of the present invention, operating process are simple and convenient.
3, the mustard oil nano-emulsion that prepared by the present invention improves the abnormal smells from the patient of stimulation, avoids volatilization, facilitates its application in practical field.
Accompanying drawing explanation
Fig. 1 embodiment 1 nano-emulsion particle size distribution.
Fig. 2 embodiment 2 nano-emulsion particle size distribution.
Fig. 3 embodiment 3 nano-emulsion particle size distribution.
Fig. 4 embodiment 4 nano-emulsion particle size distribution.
Fig. 5 embodiment 5 nano-emulsion particle size distribution.
Fig. 6 embodiment 6 nano-emulsion particle size distribution.
Detailed description of the invention
Embodiment 1:
Take polyoxyethylene hydrogenated Oleum Ricini RH405.25g, ethanol 1.75g, mustard oil 1.0g.In thermostat water bath, set temperature 50 DEG C, heats 30 minutes by polyoxyethylene hydrogenated Oleum Ricini RH40, makes it become thick liquid by paste; On magnetic stirring apparatus by polyoxyethylene hydrogenated Oleum Ricini RH40 and absolute ethyl alcohol and stirring even; Under room temperature, mustard oil is directly joined surfactant mutually in, ultrasonic disperse 3 times, each 3 minutes, at every turn ultrasonic interval was 5 minutes; In above-mentioned mixed liquor, add ultra-pure water to 500ml with constant flow pump, stir on magnetic stirring apparatus simultaneously.Constant flow pump flow velocity is set to 0.8ml/min, and agitator speed is set to 400r/min, can obtain the nano-emulsion of blue-tinted transparent shape.The concentration of mustard oil in nano-emulsion is 2.0mg/ml, and nano-emulsion mean diameter is 246.5nm.
Embodiment 2:
Take polyoxyethylene hydrogenated Oleum Ricini RH406.0g, ethanol 3.0g, mustard oil 0.6g, oleic acid 0.4g.In thermostat water bath, set temperature 55 DEG C, heats 30 minutes by polyoxyethylene hydrogenated Oleum Ricini RH40, makes it become thick liquid by paste; On magnetic stirring apparatus by polyoxyethylene hydrogenated Oleum Ricini RH40 and absolute ethyl alcohol and stirring even; Under room temperature, the oleic acid solutions being dissolved with mustard oil is directly joined surfactant mutually in, ultrasonic disperse 3 times, each 3 minutes, at every turn ultrasonic interval was 4 minutes; In above-mentioned mixed liquor, add ultra-pure water to 150ml with constant flow pump, stir on magnetic stirring apparatus simultaneously.Constant flow pump flow velocity is set to 1.0ml/min, and agitator speed is set to 450r/min, can obtain the nano-emulsion of blue-tinted transparent shape.The concentration of mustard oil in nano-emulsion is 4.0mg/ml, and nano-emulsion mean diameter is 14.45nm.
Embodiment 3:
Take lecithin 4.0g, ethanol 4.0g, mustard oil 0.8g, oleic acid 0.2g.In thermostat water bath, set temperature 60 DEG C, heats 30 minutes by lecithin, make it become thick liquid by paste; On magnetic stirring apparatus by lecithin and absolute ethyl alcohol and stirring even; Under room temperature, the oleic acid solutions being dissolved with mustard oil is directly joined surfactant mutually in, ultrasonic disperse 2 times, each 2 minutes, at every turn ultrasonic interval was 5 minutes; In above-mentioned mixed liquor, add ultra-pure water to 100ml with constant flow pump, stir on magnetic stirring apparatus simultaneously.Constant flow pump flow velocity is set to 1.2ml/min, and agitator speed is set to 500r/min, can obtain the nano-emulsion of blue-tinted transparent shape.The concentration of mustard oil in nano-emulsion is 8.0mg/ml, and nano-emulsion mean diameter is 16.23nm.
Embodiment 4:
Take poloxamer 5.25g, n-butyl alcohol 1.75g, mustard oil 1.0g.In thermostat water bath, set temperature 55 DEG C, heats 50 minutes by poloxamer, make it become thick liquid by paste; Poloxamer and n-butyl alcohol stir by magnetic stirring apparatus; Under room temperature, mustard oil is directly joined surfactant mutually in, ultrasonic disperse 3 times, each 2 minutes, at every turn ultrasonic interval was 5 minutes.In above-mentioned mixed liquor, add ultra-pure water to 100ml with constant flow pump, stir on magnetic stirring apparatus simultaneously.Constant flow pump flow velocity is set to 1.5ml/min, and agitator speed is set to 500r/min, can obtain the nano-emulsion of blue-tinted transparent shape.The concentration of mustard oil in nano-emulsion is 10.0mg/ml, and nano-emulsion mean diameter is 14.58nm.
Embodiment 5:
Take polyoxyethylene hydrogenated Oleum Ricini RH405.33g, n-butyl alcohol 2.67g, mustard oil 0.8g, oleic acid 0.2g.In thermostat water bath, set temperature 60 DEG C, heats 30 minutes by polyoxyethylene hydrogenated Oleum Ricini RH40, makes it become thick liquid by paste; Polyoxyethylene hydrogenated Oleum Ricini RH40 and n-butyl alcohol stir by magnetic stirring apparatus; Under room temperature, the oleic acid solutions being dissolved with mustard oil is directly joined surfactant mutually in, ultrasonic disperse 2 times, each 3 minutes, at every turn ultrasonic interval was 5 minutes.In above-mentioned mixed liquor, add ultra-pure water to 53ml with constant flow pump, stir on magnetic stirring apparatus simultaneously.Constant flow pump flow velocity is set to 1.8ml/min, and agitator speed is set to 500r/min, can obtain the nano-emulsion of blue-tinted transparent shape.The concentration of mustard oil in nano-emulsion is 15.0mg/ml, and nano-emulsion mean diameter is 13.36nm.
Embodiment 6:
Take polyoxyethylene hydrogenated Oleum Ricini RH404.5g, n-butyl alcohol 4.5g, mustard oil 1.0g.In thermostat water bath, set temperature 50 DEG C, heats 30 minutes by polyoxyethylene hydrogenated Oleum Ricini RH40, makes it become thick liquid by paste; Polyoxyethylene hydrogenated Oleum Ricini RH40 and n-butyl alcohol stir by magnetic stirring apparatus; Under room temperature, mustard oil is directly joined surfactant mutually in, ultrasonic disperse 3 times, each 2 minutes, at every turn ultrasonic interval was 4 minutes; In above-mentioned mixed liquor, add ultra-pure water to 50ml with constant flow pump, stir on magnetic stirring apparatus simultaneously.Constant flow pump flow velocity is set to 2.0ml/min, and agitator speed is set to 500r/min, can obtain the nano-emulsion of blue-tinted transparent shape.The concentration of mustard oil in nano-emulsion is 20.0mg/ml, and nano-emulsion mean diameter is 14.44nm.
Embodiment 7: mustard oil nano-emulsion anti-microbial property experiment of the present invention:
Laboratory sample: by the nano-emulsion obtained by embodiment 1 ~ 6.
Experimental strain: penicillium sp (CMCCF4077), aspergillus niger (ATCC16404).
Experimental technique and result:
A () bacterium liquid prepares: with inoculating loop, the strain inoculation of preservation is cultivated 24h at 37 DEG C to LB solid medium in incubator.Get the colony inoculation that grown in LB fluid medium, shaken cultivation 24h in liquid medium within, then with LB fluid medium, bacterium liquid being diluted to bacterial concentration is 10
8cfu/mL (under visible spectrophotometer, 660nm wavelength tests OD value for 0.068-0.075).
B () gets above-mentioned ready bacterium liquid 100
μl, is coated with rod with glass and is spread evenly across LB solid medium.Be the corner that the filter disc of 6mm is placed in vaccinated culture dish by diameter, then get 10
μsample drop in L embodiment 1 ~ 6 is on filter disc, and every block plate arranges a contrast, performs labelling.Culture dish is inverted, is placed in constant incubator 37 DEG C and cultivates 24h or 48h.
C () then takes out flat board, measure the size of antibacterial circle diameter around each filter paper.
Experimental result shows, the nano-emulsion obtained by embodiment 1 ~ 6 all has excellent antibacterial effect to penicillium sp and aspergillus niger.Mustard oil concentration is that the inhibition zone size of nano-emulsion to penicillium sp of 2.0mg/ml, 4.0mg/ml, 8.0mg/ml, 10.0mg/ml, 15.0mg/ml, 20.0mg/ml is respectively 2.5mm, 2.8mm, 3.2mm, 3.8mm, 5.7mm, 7.4mm; 3.2mm, 3.7mm, 4.6mm are respectively, 5.4mm, 6.9mm, 9.1mm to the inhibition zone size of aspergillus niger.
Claims (3)
1. a mustard oil nano-emulsion, it is characterized in that, by surfactant phase, oil phase and aqueous phase composition, its mass percent consists of: surfactant accounts for 1.38% ~ 22.5% mutually, oil phase accounts for 0.196% ~ 2.63%, aqueous phase accounts for 75% ~ 98.4%, wherein surfactant comprises primary surfactant and cosurfactant mutually, described primary surfactant is selected from polyoxyethylene hydrogenated Oleum Ricini RH40, lecithin, more than one mixture in poloxamer, described cosurfactant is selected from ethanol, propanol, isopropyl alcohol, more than one mixture in n-butyl alcohol or isobutanol, the mass ratio of primary surfactant and cosurfactant is 3:1 ~ 1:1, oil phase is mustard oil or the oleic acid solutions being dissolved with mustard oil.
2. the preparation method of mustard oil nano-emulsion described in claim 1, is characterized in that, comprise the following steps:
(1) preparation of surfactant
By primary surfactant in 50 ~ 60 DEG C of heating 30 ~ 60 minutes, it is made to become thick liquid by paste; Add cosurfactant again to stir, seal stand-by, described primary surfactant is selected from more than one the mixture in polyoxyethylene hydrogenated Oleum Ricini RH40, lecithin, poloxamer, and described cosurfactant is selected from more than one the mixture in ethanol, propanol, isopropyl alcohol, n-butyl alcohol or isobutanol;
(2) preparation of the oleic acid solutions of mustard oil
Under room temperature, mustard oil is joined in oleic acid, shake up to transparence, have no obvious two phase stratification phenomenon, stand-by;
(3) directly by mustard oil or in the oleic acid solutions being dissolved with mustard oil prepared in step (2) being joined surfactant that step (1) prepares, ultrasonic disperse 1 ~ 3 time, each 3 ~ 5 minutes, at every turn ultrasonic interval was 2 ~ 5 minutes;
(4) add ultra-pure water in the system obtained to step (3) with constant flow pump, stir on magnetic stirring apparatus, constant flow pump flow velocity is set to 0.8 ~ 2.0ml/min, and agitator speed is set to 400 ~ 600r/min, can obtain the nano-emulsion of blue-tinted transparent shape simultaneously.
3. preparation method according to claim 2, is characterized in that, preparation-obtained mustard oil nano-emulsion particle diameter is 13.36 ~ 246.5nm.
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| CN106333353A (en) * | 2016-08-25 | 2017-01-18 | 江南大学 | High-stability mustard oil nanometer emulsion and preparation method thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102277227A (en) * | 2010-06-13 | 2011-12-14 | 宏芳香料（昆山）有限公司 | Method for extracting mustard oil and mustard essential oil from mustard seeds |
| CN102406041A (en) * | 2011-11-29 | 2012-04-11 | 内蒙古伊利实业集团股份有限公司 | Frozen beverage added with mustard oil and preparation method of frozen beverage |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102277227A (en) * | 2010-06-13 | 2011-12-14 | 宏芳香料（昆山）有限公司 | Method for extracting mustard oil and mustard essential oil from mustard seeds |
| CN102406041A (en) * | 2011-11-29 | 2012-04-11 | 内蒙古伊利实业集团股份有限公司 | Frozen beverage added with mustard oil and preparation method of frozen beverage |
Non-Patent Citations (2)
| Title |
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| 以大豆分离蛋白为壁材喷雾干燥法制备芥末油微胶囊;盖旭等;《中国调味品》;20121231;第37卷(第3期);72-75 * |
| 大豆分离蛋白-海藻酸钠复凝聚法制备芥末油微胶囊;盖旭等;《中国调味品》;20121231;第37卷(第2期);51-54 * |
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