CN105784750A - Method of utilizing low-field nuclear magnetism to detect oil content of Euphausia superba microcapsules - Google Patents
Method of utilizing low-field nuclear magnetism to detect oil content of Euphausia superba microcapsules Download PDFInfo
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Abstract
The invention provides a method of utilizing low-field nuclear magnetism to detect oil content of Euphausia superba microcapsules. The method particularly includes: adopting low-field nuclear magnetic resonance technology to detect CPMG data of Euphausia superba microcapsule samples; utilizing a Soxhlet extraction method to obtain actual oil content of the Euphausia superba microcapsule samples; corresponding the CMPG data of the Euphausia superba microcapsule samples to the actual oil content to obtain a regression equation of Euphausia superba microcapsule oil content; acquiring CMPG data of an unknown Euphausia superba microcapsule sample, substituting into the regression equation of the Euphausia superba microcapsule oil content obtained in the step S4 to obtain oil content of the unknown Euphausia superba microcapsule sample to realize quick measuring of the oil content of the Euphausia superba microcapsule sample. By using the method, detection accuracy and accuracy of the Euphausia superba microcapsule oil content are improved greatly, and lossless, realtime and quick detection is realized.
Description
Technical field
The present invention relates to a kind of Antarctic krill microcapsule oil content detection method field, particularly to the method utilizing low field nuclear-magnetism detection Antarctic krill microcapsule oil content.
Background technology
Antarctic krill is just receiving the concern of more and more national as a kind of highly important fishery resources.At present, antarctic krill oil (KrillOil) is Related product Middle nutrition effect and all significantly high product of added value.Antarctic krill oil is the complex of its lipid component, except main fatty acid and each analog derivative thereof, possibly together with some other liposoluble substances, such as astaxanthin, vitamin, sterol etc.；Positive and negative synergism just because of different kinds of molecules just creates unique effect.
Microcapsule technology, be a kind of adopt natural or synthesis macromolecular material solid or liquid are made the technology with the miniature tolerant of polymeric shell wall or packing material.Currently, with respect to the report of grease microcapsule, it is mostly the research about microcapsule preparation method.And microcapsule oil content is the key factor affecting its quality.The oil content of microcapsule finished product there is significantly high requirement by the series of processes prepare grease microcapsule.Measure grease microcapsule oil content rapidly and accurately and prepare significant for the production of Antarctic krill microcapsule.
Currently, with respect to the research of quickly detection of oil content of Antarctic krill microcapsule, there is not been reported.The common method being generally used for oil content analysis has soxhlet extraction methods and spectrophotography.In actual use, result is inaccurate, analysis process is consuming time and uses the problems such as substantial amounts of toxic organic solvents in said method existence analysis.Scholar was had to utilize near-infrared spectral analysis technology that the oil content of instant noodles is measured research in recent years, although this method can measure Antarctic krill microcapsule sample oil content to a certain extent, but it is the damageability of sample is big, it is impossible to ensure the integrity of sample, have certain limitation.Therefore, in the urgent need to a kind of method of Fast nondestructive evaluation Antarctic krill microcapsule oil content.
The ultimate principle of low-field nuclear magnetic resonance (LF-NMR) is by the sample being in stationary magnetic field is applied radio-frequency pulse, Hydrogen Proton is made to resonate, proton discharges the rf wave energy absorbed and returns to ground state in radiationless mode, and this process is relaxation process.Difference according to energy exchange object, relaxation process can be divided into transverse relaxation and longitudinal relaxation, and the corresponding relaxation time represents with T2 and T1 respectively.The length in relaxation time is relevant with residing physicochemical environment with the existence of sample interior Hydrogen Proton, and the intensity of relaxation signals is relevant to Hydrogen Proton number in sample.
Summary of the invention
The discriminating of Antarctic krill microcapsule quality has very important significance, present invention aim at, for Antarctic krill microcapsule oil content analyze inaccurate, analysis process is consuming time and the problem that uses substantial amounts of toxic organic solvents, there is provided a kind of simple, quickly, accurately, the method for the detection Antarctic krill microcapsule oil content of environmental protection, reduce testing cost simultaneously, fully ensure that the quality of Antarctic krill microcapsule.
For reaching above-mentioned purpose, the invention provides a kind of method utilizing low field nuclear-magnetism detection Antarctic krill microcapsule oil content, specifically comprise the following steps that
S1, taking six groups of Antarctic krill oil microcapsule samples that theoretical oil content is 10%, 20%, 30%, 40%, 50%, 60%, often group three is parallel, and each parallel 20.00 ± 0.05g that weighs is as detection sample, standby；
The CPMG data of each Antarctic krill microcapsule sample that S2, employing low-field nuclear magnetic resonance technology for detection step S1 obtain；
The CPMG sequence parameter of described low field nmr analysis is: 90 degree of pulsewidth P1:13 μ s, 180 degree of pulsewidth P2:26 μ s, repeated sampling waiting time Tw:2000ms, analog gain RG1:20, digital gain DRG1:3, pre-amp gain PRG:3, repeated sampling times N S:8, echo number NECH:2000, receiver bandwidth SW:100KHz, the control parameter RFD:0.2ms, time delay D L1:0.5ms that start the sampling time carry out NMR signal collection；
S3, soxhlet extraction is utilized to extract the oils and fats of each Antarctic krill microcapsule sample after step S2 detects, it is thus achieved that the actual oil content of described each Antarctic krill microcapsule sample；
S4, the actual oil content of described each Antarctic krill microcapsule sample that the CMPG data of the described each Antarctic krill microcapsule sample obtained by step S2 obtain with step S3 are corresponding, employing partial least-square regression method processes, obtain residual variance because of the regression equation of subnumber collection of illustrative plates and Antarctic krill microcapsule oil content, take 4 main constituents because of subnumber, set up Antarctic krill microcapsule oil content test database；
S5, the method identical with step S2 is adopted to obtain the CMPG data of the unknown Antarctic krill microcapsule sample, it is conducted in Unscrambler software, choose " Predict " pattern, substitute into the regression equation of the step S4 Antarctic krill microcapsule oil content obtained, the described Antarctic krill microcapsule oil content test database that invocation step S4 sets up, obtain the oil content of described unknown Antarctic krill microcapsule sample, it is achieved the quick mensuration of unknown Antarctic krill microcapsule sample oil content.
Under optimal way, extract the oils and fats of Antarctic krill microcapsule sample described in step S3, it is thus achieved that oil content method particularly includes: accurately weigh 2.00 ± 0.05g microcapsule sample and record weighing value (m0), it is encased in fat-free filter paper, then is put in the apparatus,Soxhlet's of known weight, utilize apparatus,Soxhlet's reflux, extract, 6h in the petroleum ether of 65 DEG C, then 105 DEG C of drying obtain total oil quality (m) to constant weight weighing, the two mass ratio (m/m0) it is microcapsule sample oil content.
The advantage of the present invention:
1, the method for the present invention does not have the sample pretreatment process of complexity, can realize the quickly detection of Antarctic krill microcapsule oil content and analyze, thus the quality of the Antarctic krill microcapsule prepared quickly is identified within a few minutes.Compared with traditional method, the inventive method not only increases detection speed, and the accuracy detected also is greatly improved.
2, compared with traditional method, the inventive method analyzes that result is accurate, and reproducible, analysis time is short, less than 5min, to sample without destruction, for non-intrusion measurement method, and avoids the use of a large amount of organic reagent.
3, the present invention rationally determines modeling main cause subnumber, takes full advantage of spectral information filter out noise, makes testing result more accurate.
4, under normal circumstances, the oil content of Antarctic krill microcapsule is 1%～55%, and the inventive method is chosen the Antarctic krill microcapsule sample that theoretical oil content is 10～60% and is modeled, and has simplified modeling process, simultaneously, it is ensured that precision of analysis.
The present invention is fully recognized that the importance of Antarctic krill microcapsule quality discernment, is greatly improved detection speed and accuracy, realize simultaneously lossless, real-time, quickly detect.The inventive method can be applicable to the content measurement of the Antarctic krill microcapsule oil of different preparation method gained, and measurement result accuracy is high, reproducible, consuming time short.
Accompanying drawing explanation
Fig. 1 is the CPMG attenuation curve spectrogram of Antarctic krill microcapsule；
Fig. 2 is the transverse relaxation T2 spectrogram of detection Antarctic krill microcapsule；
Fig. 3 be in calibration set the residual variance of Antarctic krill microcapsule oil content because of subnumber；
Fig. 4 is the recurrence spectrogram of calibration set Antarctic krill microcapsule oil content practical measurement value and predictive value；
Fig. 5 is the recurrence spectrogram of validation-cross collection Antarctic krill microcapsule oil content practical measurement value and predictive value；
Fig. 6 is the standard deviation spectrogram of the offset minimum binary of the oil content of calibration set and validation-cross collection Antarctic krill microcapsule.
Detailed description of the invention
In order to make those skilled in the art be better understood from the present invention, below in conjunction with detailed description of the invention, the present invention is further described.
Embodiment:
One, the magnetic resonance relaxation spectrum of Antarctic krill microcapsule sample is analyzed
The Antarctic krill microcapsule sample of the different core wall ratio of preparation, owing to the core wall ratio of Antarctic krill microcapsule sample is different, its oil content also differs accordingly.Taking six groups of Antarctic krill oil microcapsule samples that theoretical oil content is 10%, 20%, 30%, 40%, 50%, 60%, often group three is parallel, and each parallel 2.00 ± 0.05g that weighs is as detection sample, totally 18 Antarctic krill microcapsule samples.nullAdopt MiniMR-Rat magnetic resonance imaging analysis instrument，Utilize multiple-pulse spin-echo sequence (Carr-Purcell-Meiboom-Gill (CPMG) sequence)，Measure Antarctic krill microcapsule sample T2 T2，Parameter is set to: 90 degree of pulsewidth P1:13 μ s，180 degree of pulsewidth P2:26 μ s，Repeated sampling waiting time Tw:2000ms，Analog gain RG1:20，Digital gain DRG1:3，Pre-amp gain PRG:3，NS:8，NECH:2000，Receiver bandwidth SW:100KHz，Start the control parameter RFD:0.2ms in sampling time，Time delay D L1:0.5ms carries out NMR signal collection，Draw CPMG decay collection of illustrative plates (Fig. 1) of each sample.
The Antarctic krill microcapsule sample that core ratio is more high as seen from Figure 1, its decay is more slow, and this can illustrate that Antarctic krill microcapsule sample oil content is of a relatively high.
Then adopt one-dimensional anti-Laplacian algorithm as T2 T2 inversion algorithm (iterations: 1000000), draw transverse relaxation characteristic collection of illustrative plates (Fig. 2) of each sample.
In Fig. 2, T22 and T23 is regarded as oils and fats peak in Antarctic krill microcapsule sample.The sample that the gross area of A22 and the A23 of the Antarctic krill microcapsule sample that fat content is high is low more than fat content is can be seen that from Fig. 2 spectrogram.
Two, the oil content forecast model of Antarctic krill microcapsule sample
Obtain the actual oil content of 18 Antarctic krill microcapsule samples according to soxhlet extraction, result is as shown in table 1.
The detection method of above-mentioned six groups of actual oil contents of Antarctic krill oil microcapsule is:
Accurately weigh 2.00 ± 0.05g microcapsule sample and record weighing value (m0), it is encased in fat-free filter paper, then is put in the apparatus,Soxhlet's of known weight, utilize apparatus,Soxhlet's reflux, extract, 6h in the petroleum ether of 65 DEG C, then 105 DEG C of constant weights weighing obtain total oil quality (m), the two mass ratio (m/m0) it is microcapsule sample oil content.
Calculating process for theoretical oil content be 10%, the Antarctic krill microcapsule sample of numbering 1, weigh m0For 2.0212g, after Soxhlet extraction, total oil quality m is 0.0296, and oil content is:
(0.0296/2.0212) * 100%=1.46%
The actual oil content of table 1 Antarctic krill microcapsule sample
In order to obtain the forecast model of oil content further, by the value of the transverse relaxation data of Antarctic krill microcapsule sample and the oil content of practical measurement, jointly it is analyzed in conjunction with partial least-squares regressive analysis method.Fig. 3 be in calibration set the residual variance of Antarctic krill microcapsule oil content because of subnumber；From figure 3, it can be seen that optimum factor number is 4.In order to obtain forecast model accurately, choose 4 main constituents because of subnumber so that residual deviation value is minimum.
Finally, the regression equation according to oil content in table 1 and CMPG data acquisition Antarctic krill microcapsule oil content: calibration model and validation-cross model (Fig. 4 and Fig. 5), it is achieved the fast prediction of Antarctic krill microcapsule oil content.
The scatter plot distributions ratio of microcapsule sample oil content can be will become apparent from more uniform from Fig. 4 and Fig. 5.The result of calibration set and validation-cross collection is close, coefficient R cal2And Rcv2Respectively 0.9800 and 0.9680, it is all higher than 0.85, root-mean-square error RMSEC and RMSECV respectively 0.0262 and 0.0332, all less, illustrate that low-field nuclear magnetic resonance can microcapsule oil content exactly in conjunction with PCR.
In order to evaluate the forecast model of Antarctic krill microcapsule oil content further, the present invention can also pass through outside the data evaluation of table 2, also to investigate the tightness degree of scatterplot in the spectrogram (Fig. 6) of residual error, more tight, it is more accurate that forecast model is predicted, residual error is distributed between-2 and 2, and scatterplot is very tight, illustrates that the modelling effect set up is good.
The data of the PLS that table 2 is analyzed based on original and fitting data
Three, the unknown Antarctic krill microcapsule oil content of oil content forecast model detection of Antarctic krill microcapsule sample is utilized
The method identical with detection test specimens is adopted to obtain the CMPG data of unknown Antarctic krill microcapsule sample, substitute into the regression equation of Antarctic krill microcapsule oil content, obtain the oil content of described unknown Antarctic krill microcapsule sample, it is achieved the quick mensuration of unknown Antarctic krill microcapsule sample oil content.
Fig. 4 calibration model obtained above is forecast model, and Fig. 5 validation-cross is generally used to the Stability and veracity that inspection calibration model predicts the outcome.
Table 3 is the comparison of the actual value of unknown Antarctic krill microcapsule sample oil content and predictive value, and described unknown Antarctic krill microcapsule sample oil content actual value is to adopt the method acquisition identical with above-mentioned test specimens；Predictive value preparation method is first to put into unknown sample in the nuclear-magnetism of low field to scan, it is thus achieved that CMPG data, then is conducted in Unscrambler software, utilizes the model having built up, obtains corresponding oil content predictive value.
The actual value of the unknown Antarctic krill microcapsule sample oil content of table 3 and the comparison of predictive value
Relative Error is the relative error between actual value and predictive value, from table 3 it can be seen that the forecast model relative error that application the inventive method is set up is very little, this further illustrates the inventive method and analyzes result accurately, reproducible.
The above; it is only the present invention preferably detailed description of the invention; but protection scope of the present invention is not limited thereto; any those familiar with the art is in the technical scope of present disclosure; it is equal to replacement according to technical scheme and inventive concept thereof or is changed, all should be encompassed within protection scope of the present invention.
Claims (2)
1. the method utilizing low field nuclear-magnetism detection Antarctic krill microcapsule oil content, it is characterised in that specifically comprise the following steps that
S1, taking six groups of Antarctic krill oil microcapsule samples that theoretical oil content is 10%, 20%, 30%, 40%, 50%, 60%, often group three is parallel, and each parallel 20.00 ± 0.05g that weighs is as detection sample, standby；
The CPMG data of each Antarctic krill microcapsule sample that S2, employing low-field nuclear magnetic resonance technology for detection step S1 obtain；
The CPMG sequence parameter of described low field nmr analysis is: 90 degree of pulsewidth P1:13 μ s, 180 degree of pulsewidth P2:26 μ s, repeated sampling waiting time Tw:2000ms, analog gain RG1:20, digital gain DRG1:3, pre-amp gain PRG:3, repeated sampling times N S:8, echo number NECH:2000, receiver bandwidth SW:100KHz, the control parameter RFD:0.2ms, time delay D L1:0.5ms that start the sampling time carry out NMR signal collection；
S3, soxhlet extraction is utilized to extract the oils and fats of each Antarctic krill microcapsule sample after step S2 detects, it is thus achieved that the actual oil content of described each Antarctic krill microcapsule sample；
S4, the actual oil content of described each Antarctic krill microcapsule sample that the CMPG data of the described each Antarctic krill microcapsule sample obtained by step S2 obtain with step S3 are corresponding, employing partial least-square regression method processes, obtain residual variance because of the regression equation of subnumber collection of illustrative plates and Antarctic krill microcapsule oil content, take 4 main constituents because of subnumber, set up Antarctic krill microcapsule oil content test database；
S5, the method identical with step S2 is adopted to obtain the CMPG data of the unknown Antarctic krill microcapsule sample, it is conducted in Unscrambler software, choose " Predict " pattern, substitute into the regression equation of the step S4 Antarctic krill microcapsule oil content obtained, the described Antarctic krill microcapsule oil content test database that invocation step S4 sets up, obtain the oil content of described unknown Antarctic krill microcapsule sample, it is achieved the quick mensuration of unknown Antarctic krill microcapsule sample oil content.
2. the method utilizing low field nmr analysis Antarctic krill microcapsule oil content according to claim 1, it is characterized in that, the oils and fats of Antarctic krill microcapsule sample is extracted described in step S3, obtain oil content method particularly includes: accurately weigh 2.00 ± 0.05g microcapsule sample and record weighing value, it is encased in fat-free filter paper, it is put into again in the apparatus,Soxhlet's of known weight, utilize apparatus,Soxhlet's reflux, extract, 6h in the petroleum ether of 65 DEG C, then 105 DEG C of drying obtain total oil quality to constant weight weighing, the two mass ratio is the oil content of described Antarctic krill microcapsule sample.
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