CN103940783A - Method for predicting shelf-life stability of sterilized milk - Google Patents
Method for predicting shelf-life stability of sterilized milk Download PDFInfo
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- CN103940783A CN103940783A CN201410186951.2A CN201410186951A CN103940783A CN 103940783 A CN103940783 A CN 103940783A CN 201410186951 A CN201410186951 A CN 201410186951A CN 103940783 A CN103940783 A CN 103940783A
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Abstract
The invention discloses a method for predicting the shelf-life stability of sterilized milk. The method comprises the following steps: (1) scanning and measuring the average back scattering light change rate of the sterilizer milk within 22-26 hours in a stability analyzer under aseptic operation, and analyzing data of the average scattering light change rate to obtain an STI value; (2) judging the shelf-life stability of the sterilized milk according to the STI value, when the STI value is less than 1.5, judging that the sterilized milk is accordant with the shelf life of 6 months, when the STI value is more than or equal to 1.5 and less than 2, judging that the sterilized milk is not accordant with the shelf life of 6 months, and when the STI value is more than or equal to 2, judging that the shelf life of the sterilized milk is less than 150 days, wherein the temperature in the scanning and measuring process is 25-40 DEG C. By adopting the method, relevant analysis can be finished within 26 hours, and the shelf-life stability of the sterilized milk can pre-judged rapidly and accurately. The method is very convenient and practical.
Description
Technical field
The present invention relates to a kind of method of predicting sterile milk shelf-life internal stability.
Background technology
Milk is rich in the nutritions such as mineral matter, vitamin, protein, fat because of it, be a kind of well food.But because of its complicated component, long-time preservation is also very difficult.Although solved the pollution of microorganism through ultrapasteurized product, the unstable of proterties also can occur, as phenomenons such as fat floating, protein micelle flocculation sediments.Ultra high temperature sterilization (UHTS) milk is according to the difference of packaging material, and shelf life can reach 2-6 month.When the long shelf life later stage, milk may occur that the impacts such as fat floating are tasted and the phenomenon of sense organ.The stability performance of its shelf life of milk of different pastures or Various Seasonal is also different.Its influence factor complexity, comprises the situations such as the microorganism, lipase, concentration of metal ions of raw material milk.In actual production, be difficult to the composition that may affect stability in raw material milk to carry out item by item express-analysis detection, the time cost doing like this and testing cost are that factory is difficult to bear.From some documents, we can know that scientific experiments of some research milk unstable reasons carry out, but not about the method for quick anticipation the stability of milk.
The stability factor aspect of emulsion is devoted in current correlative study mostly, the technology that is generally used for detecting emulsion stability has two kinds, one is directly to observe by eyes, and another is to adopt analytical instrument to detect (laser particle size analysis method, microscopic examination method, flow graph etc.).External scientist is by the loss effect of optical microscope and flow graph checking milk emulsion flocculate, study emulsion precipitation rising phenomenon by adding the casein sodium of various dose, experimental results show that casein sodium micella can cause that emulsion drop produces vacancy flocculation.Some research shows to improve milk protein concentration can stable colloid system liquid level and fat globule interface, and this physical treatment method can cause the unstable of emulsion, such as the phenomenon such as fat floating, flocculation.These phenomenons also belong to the unstable performance of long shelf life milk just.But detect this emulsion drop instable layer analytical approach also under study for action, cannot accomplish quick anticipation.In classic method, judge its stability by visual inspection and accelerated test, this needs for a long time and result seriously lags behind, and the instrument tests such as employing laser particle size analyzer, microscope, can not set up a criterion fast and accurately, be difficult to accomplish superhigh temperature milk shelf stable is carried out to anticipation.
In prior art, also useful stability analysis instrument is analyzed the stability of anticipation long shelf life milk.Use Turbiscan analyser to test sample stability, testing sample is contained in a columniform glass test cabinet, instrument adopts pulse near-infrared light source (λ=880nm), when an electromagnetic wave is transmitted into while being contained in the poor detection sample of the transparency of glass test cabinet, Turbiscan analyser can obtain dimeric launch spot, and two synchronous optical detectors are surveyed respectively through the transmitted light of sample and the reflected light that reflected by sample.Transmitted light and reflected light represent with %, and its implication is the number percent of the luminous flux of relative standard's sample.Scanning curve has provided transmitted light and the reflected light variation relation with height of specimen.These curves have reflected microscopic feature within preset time.Conventionally, transmission to muddy sample, is used for analyze opaque sample and reflect for transparent, and sterile milk belongs to opaque system.Tested sample concentration is constant, transmitted light and catoptrical changing value are Delta Transmission (△ T so, %) and DeltaBackscattering (△ BS, %), directly reflected particle rule over time in sample.According to multiple Scattering principle, on the basis of light intensity, can calculate floating layer, the beds of precipitation thickness temporal evolution situation of sample.△ BS and system stability are negative correlation, and △ BS value is less, more stable with regard to expression system, and △ BS is worth larger, more unstable with regard to expression system.In prior art, there is the △ BS value under the different temperatures measured, use the △ BS value under these different temperatures to set up linear equation, and calculate the △ BS value under two different temperatures of actual needs according to linear equation, speed-up ratio (Accelerated Ration using both ratios as sterile milk shelf life accelerated test, AR), then after measuring actual shelf-life of the lower sterile milk that (is generally 30-50 DEG C) under higher temperatures environment, be multiplied by this speed-up ratio, draw the shelf-life of (being generally 25 DEG C) at the temperature needing.But the method, need to measure the actual shelf-life under higher temperatures, also need 1-3 month, process is not only long but also loaded down with trivial details, and available accuracy is not very high.
Summary of the invention
The technical matters that the present invention solves is very length, the not high defect of accuracy of method time of surveying sterile milk shelf-life internal stability in prior art in order to overcome, and a kind of method of brand-new prediction sterile milk shelf-life internal stability is provided.This method can complete correlation analysis in 26 hours, can make anticipation to the shelf stable of sterile milk rapidly and accurately, very convenient practicality.
The invention provides a kind of method of predicting sterile milk shelf-life internal stability, it comprises the steps:
(1) by sterile milk under sterile working, in stability analysis instrument, the average backscattered light rate of change (△ BS) of scanning survey sterile milk in 22-26 hour, the data of described average scattering light rate of change (△ BS) draw stability kinetic parameter (STI) value by analysis; (2) be worth according to stability kinetic parameter (STI) the shelf-life stability that judges sterile milk; As described STI value < 1.5, the described sterile milk of judgement meets 6 months shelf-lifves; When described STI value is 1.5≤STI value < 2, the described sterile milk of judgement does not meet 6 months shelf-lifves; When described STI value >=2, judge that the shelf-life of described sterile milk is less than 150 days; Wherein, the temperature in described scanning survey process is 25-40 DEG C.
It should be noted that, before the present invention, in the middle of sterile milk, generally all use stabilizing agent, time shelf-life is longer, the foundation of kinetic parameter model is also more ripe, but national food safety standard regulation sterile milk of today can not use food additives, equal sterile milk system and of the prior art completely different, sterile milk becomes the system of a sealing relatively, can only rely on the stability of inner eggs white gel bundle to provide support.In order to adapt to brand-new sterile milk system, inventor is through test of long duration, unexpected find to use the specific operation of the present invention and step, by analyzing the initial STI value of sterile milk, can dope rapidly and accurately the stability during shelf-life and shelf-life of sterile milk.
In the present invention, described sterile milk is the sterile milk of this area routine, according to the sterile milk of the categorised regulation of " sterile milk " in national standard.Described breast is preferably that cow's milk, sheep breast or cattle and sheep mix breast, is more preferably cow's milk.Described cow's milk leading indicator is: fat (F) content >=3.1%, protein (P) content >=2.9%, non-fat solid (SNF) >=8.1%.
In the present invention, described sterile milk is generally highly put into described stability analysis instrument according to the addition of the sterile milk sample of this area routine and interpolation.The addition of described sterile milk is preferably 20.0ml, and the interpolation of described sterile milk is highly preferably 45.0mm.
In the present invention, described stability analysis instrument be this area routine for analyzing the stability analysis instrument of the average backscattered light rate of change of sterile milk, being preferably Turbiscan stability analysis instrument, is more preferably the Turbiscan stability analysis instrument that French Formulaction company produces.
Temperature in described scanning survey process is preferably 35 DEG C.
In the present invention, described scanning survey is the operation of this area routine, is generally according to sterile milk of certain hour interval scan, finally draws the data that in predetermined T.T., several times scanning survey draws.The time of described scanning survey sterile milk is preferably 24 hours.
In the present invention, the time interval of described scanning survey is 1-120min, is preferably 20min.
In the present invention, the analysis of the data of described average scattering light rate of change (△ BS) is to analyze by the method for this area routine, obtain stability kinetic parameter (STI=stability index) value, preferably, for analyzing through TurbiscanEasysoft software, obtain described stability kinetic parameter (STI) value.Described TurbiscanEasysoft software is this area routine, the software very generally using.STI value generally draws by setting up steady dynamic mechanics parameter evaluation model, STI=[(T
d× K)/Δ BS] × (t
d/ 24), wherein, K is constant, t
dfor the observing time of ultra-high-temperature sterilized milk; T
dstablize dynamic (dynamical) Celsius temperature for measuring ultra-high-temperature sterilized milk sample.
Meeting on the basis of this area general knowledge, above-mentioned each optimum condition, can combination in any, obtains the preferred embodiments of the invention.
Agents useful for same of the present invention and raw material be commercially available obtaining all.
Positive progressive effect of the present invention is: the inventive method can complete correlation analysis in 26 hours, can make anticipation to the shelf stable of sterile milk rapidly and accurately, very convenient practicality.
Brief description of the drawings
Fig. 1 is the residual fat deposit constitutional diagram in inner packing in the time that the shelf-life arrives of the sterile milk of embodiment 1-6 test.
Fig. 2 is the sample granularity distribution plan of sterile milk after product initial stage and 6 months of test in embodiment 1.
Fig. 3 is the sample granularity distribution plan of sterile milk after product initial stage and 6 months of test in embodiment 2.
Fig. 4 is the sample granularity distribution plan of sterile milk after product initial stage and 6 months of test in embodiment 3.
Fig. 5 is the sample granularity distribution plan of sterile milk after product initial stage and 6 months of test in embodiment 4.
Fig. 6 is the sample granularity distribution plan of sterile milk after product initial stage and 6 months of test in embodiment 5.
Fig. 7 is the sample granularity distribution plan of sterile milk after product initial stage and 6 months of test in embodiment 6.
Fig. 8 is the sample granularity distribution plan of sterile milk after product initial stage and 6 months of test in embodiment 7.
Fig. 9 is the sample granularity distribution plan of sterile milk after product initial stage and 6 months of test in comparative example 1.
Embodiment
Mode below by embodiment further illustrates the present invention, but does not therefore limit the present invention among described scope of embodiments.The experimental technique of unreceipted actual conditions in the following example, according to conventional method and condition, or selects according to catalogue.
The analytical equipment that the present invention uses is Turbiscan stability analysis instrument, French Formulaction company.
Implementation result need to by observing after accelerated test, sample or shelf-life be watched sample state while arriving and sample granularity changes in distribution situation is verified.Carry out the change of granularity of initial and shelf-life of comparative sample while finishing by size-grade distribution, the equipment of employing is Mastersizer Malvern3000 type laser particle analyzer type laser particle analyzer.
Embodiment 1
| Sample | Sample index |
| Sterile milk | Fat 3.5%, protein 2.9%, non-fat solid 8.3% |
Sample, under sterile working, is placed in to test cabinet, puts into stability analysis instrument, the addition of sterile milk sample is 20.0ml, and adding is highly 45.0mm.It is 1min that sweep spacing is set, sample chamber temperature is 35 DEG C, scanning survey 24 hours, analyze the data of the average scattering light rate of change (△ BS) in 24 hours through TurbiscanEasysoft software, obtaining stability kinetic parameter (STI) value is 0.8, judges that 6 months its shelf-lifves internal stability is good.
Implementation result: shown in Fig. 1,2 (curve A representative sample is initial, when curve B represents 6 months), it is less that the shelf-life is packed residual fat deposit while arrival, and size-grade distribution is little compared with product Initial change.Show that above-mentioned measurement result and actual shelf-life internal stability are basically identical.
Embodiment 2
| Sample | Sample index |
| Sterile milk | Fat 3.6%, protein 3.1%, non-fat solid 8.3% |
Sample, under sterile working, is placed in to test cabinet, puts into stability analysis instrument, the addition of sterile milk sample is 20.0ml, and adding is highly 45.0mm.It is 20min that sweep spacing is set, sample chamber temperature is 25 DEG C, scanning survey 24 hours, analyze the data of the average scattering light rate of change (△ BS) in 24 hours through TurbiscanEasysoft software, obtaining stability kinetic parameter (STI) value is 1.17, judges that 6 months its shelf-lifves internal stability is good.
Implementation result: shown in Fig. 1,3 (curve A representative sample is initial, when curve B represents 6 months), it is less that the shelf-life is packed residual fat deposit while arrival, and size-grade distribution is little compared with product Initial change.Show that above-mentioned measurement result and actual shelf-life internal stability are basically identical.
Embodiment 3
| Sample | Sample index |
| Sterile milk | Fat 3.5%, protein 3.0%, non-fat solid 8.4% |
Sample, under sterile working, is placed in to test cabinet, puts into stability analysis instrument, the addition of sterile milk sample is 20.0ml, and adding is highly 45.0mm.It is 120min that sweep spacing is set, sample chamber temperature is 40 DEG C, scanning survey 24 hours, analyze the data of the average scattering light rate of change (△ BS) in 24 hours through TurbiscanEasysoft software, obtaining stability kinetic parameter (STI) value is 1.25, judges that 6 months its shelf-lifves internal stability is good.
Implementation result: shown in Fig. 1,4 (curve A representative sample is initial, when curve B represents 6 months), it is less that the shelf-life is packed residual fat deposit while arrival, and size-grade distribution is little compared with product Initial change.Show that above-mentioned measurement result and actual shelf-life internal stability are basically identical.
Embodiment 4
| Sample | Sample index |
| Sterile milk | Fat 3.3%, protein 2.9%, non-fat solid 8.4% |
Sample, under sterile working, is placed in to test cabinet, puts into stability analysis instrument, the addition of sterile milk sample is 20.0ml, and adding is highly 45.0mm.It is 60min that sweep spacing is set, sample chamber temperature is 25 DEG C, scanning survey 24 hours, analyze the data of the average scattering light rate of change (△ BS) in 24 hours through TurbiscanEasysoft software, obtaining stability kinetic parameter (STI) value is 2.61, judge that its shelf-life internal stability is poor, do not reach the requirement of six months shelf-lifves, the shelf-life is less than 150 days.
Implementation result: shown in Fig. 1,5 (curve A representative sample is initial, when curve B represents 6 months), the shelf-life packs that residual fat deposit is more while arrival, curve B occurs significantly bimodal or multimodal, and size-grade distribution is larger compared with product Initial change.Show that above-mentioned measurement result and actual shelf-life internal stability are basically identical.
Embodiment 5
| Sample | Sample index |
| Sterile milk | Fat 3.2%, protein 2.9%, non-fat solid 8.4% |
Sample, under sterile working, is placed in to test cabinet, puts into stability analysis instrument, the addition of sterile milk sample is 20.0ml, and adding is highly 45.0mm.It is 30min that sweep spacing is set, sample chamber temperature is 30 DEG C, scanning survey 24 hours, analyze the data of the average scattering light rate of change (△ BS) in 24 hours through TurbiscanEasysoft software, obtaining stability kinetic parameter (STI) value is 3.66, judge that its shelf-life internal stability is poor, do not reach the requirement of six months shelf-lifves, the shelf-life is less than 150 days.
Implementation result: (curve A representative sample is initial as Fig. 1,6, when curve B represents 6 months) shown in, shelf-life packs that residual fat deposit is more, color increases the weight of while arrival, and curve B occurs significantly bimodal or multimodal, and size-grade distribution is very large compared with product Initial change.Show that above-mentioned measurement result and actual shelf-life internal stability are basically identical.
Embodiment 6
| Sample | Sample index |
| Sterile milk | Fat 3.3%, protein 2.9%, non-fat solid 8.4% |
Sample, under sterile working, is placed in to test cabinet, puts into stability analysis instrument, the addition of sterile milk sample is 20.0ml, and adding is highly 45.0mm.It is 20min that sweep spacing is set, sample chamber temperature is 35 DEG C, scanning survey 24 hours, analyze the data of the average scattering light rate of change (△ BS) in 24 hours through TurbiscanEasysoft software, obtaining stability kinetic parameter (STI) value is 4.25, judge that its shelf-life internal stability is poor, do not reach the requirement of six months shelf-lifves, the shelf-life is less than 150 days.
Implementation result: (curve A representative sample is initial as Fig. 1,7, when curve B represents 6 months) shown in, shelf-life packs that residual fat deposit is more while arrival, color has started jaundice, and curve B occurs significantly bimodal or multimodal, and size-grade distribution is very large compared with product Initial change.Show that above-mentioned measurement result and actual shelf-life internal stability are basically identical.
Embodiment 7
| Sample | Sample index |
| Sterile milk | Fat 3.4%, protein 3.0%, non-fat solid 8.4% |
Sample, under sterile working, is placed in to test cabinet, puts into stability analysis instrument, the addition of sterile milk sample is 20.0ml, and adding is highly 45.0mm.It is 20min that sweep spacing is set, sample chamber temperature is 25 DEG C, scanning survey 24 hours, analyze the data of the average scattering light rate of change (△ BS) in 24 hours through TurbiscanEasysoft software, obtaining stability kinetic parameter (STI) value is 1.89, judge that its shelf-life internal stability is poor, do not reach the requirement of six months shelf-lifves.
Implementation result: shown in Fig. 8 (curve A representative sample is initial, when curve B represents 6 months), when the shelf-life arrives, size-grade distribution is larger compared with product Initial change.Show that above-mentioned measurement result and actual shelf-life internal stability are basically identical.
Comparative example 1
| Sample | Sample index |
| Sterile milk | Fat 3.4%, protein 3.0%, non-fat solid 8.4% |
Sample, under sterile working, is placed in to test cabinet, puts into stability analysis instrument, the addition of sterile milk sample is 20.0ml, and adding is highly 45.0mm.It is 20min that sweep spacing is set, sample chamber temperature is 10 DEG C, scanning survey 24 hours, analyze the data of the average scattering light rate of change (△ BS) in 24 hours through TurbiscanEasysoft software, obtaining stability kinetic parameter (STI) value is 0.82, judges that 6 months its shelf-lifves internal stability is good.
Actual implementation result: shown in Fig. 9 (curve A representative sample is initial, when curve B represents 6 months), when the shelf-life arrives, size-grade distribution is larger compared with product Initial change.Result of determination and actual conditions are not in advance inconsistent completely.
Claims (8)
1. predict the method for sterile milk shelf-life internal stability for one kind, it is characterized in that, comprise the steps: (1) by sterile milk under sterile working, in stability analysis instrument, the average backscattered light rate of change of scanning survey sterile milk in 22-26 hour, the data of described average scattering light rate of change draw STI value by analysis; (2) judge the shelf-life stability of sterile milk according to STI value; As described STI value < 1.5, the described sterile milk of judgement meets 6 months shelf-lifves; When described STI value is 1.5≤STI value < 2, the described sterile milk of judgement does not meet 6 months shelf-lifves; When described STI value >=2, judge that the shelf-life of described sterile milk is less than 150 days; Wherein, the temperature in described scanning survey process is 25-40 DEG C.
2. the method for claim 1, is characterized in that, the temperature in described scanning survey process is 35 DEG C.
3. the method for claim 1, is characterized in that, the addition of described sterile milk is 20.0ml; With or, the interpolation of described sterile milk is highly 45.0mm.
4. the method for claim 1, is characterized in that, described stability analysis instrument is Turbiscan stability analysis instrument.
5. the method for claim 1, is characterized in that, described sterile milk is that cow's milk, sheep breast or cattle and sheep mix breast.
6. the method for claim 1, is characterized in that, the time of described scanning survey sterile milk is 24 hours; And/or the time interval of described scanning survey is 1-120min.
7. method as claimed in claim 6, is characterized in that, the time interval of described scanning survey is 20min.
8. the method for claim 1, is characterized in that, the analysis of the data of described average scattering light rate of change is to analyze through TurbiscanEasysoft software, obtains described STI value.
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| CN111766353A (en) * | 2020-06-24 | 2020-10-13 | 河北兄弟伊兰食品科技股份有限公司 | Method for rapidly judging stability of drinking yoghourt with long shelf life |
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Application publication date: 20140723 |